#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2011403.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2011403
loop_
_publ_author_name
'Cui, Yong'
'Zhang, Xing'
'Zheng, Fakun'
'Ren, Jing'
'Chen, Gang'
'Qian, Yitai'
'Huang, Jinshun'
_publ_section_title
;
 Two mixed-metal carboxylate--base adducts
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1198
_journal_page_last               1200
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Ca Zn2 (C3 H5 O2)6 (C9 H7 N)2]'
_chemical_formula_moiety         'C36 H44 Ca N2 O12 Zn2'
_chemical_formula_sum            'C36 H44 Ca N2 O12 Zn2'
_chemical_formula_weight         867.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.614(2)
_cell_length_b                   19.363(4)
_cell_length_c                   12.473(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.95
_cell_volume                     2070.5(8)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0000
_diffrn_reflns_av_sigmaI/netI    .0289
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3633
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.95
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  .875
_exptl_absorpt_correction_T_min  .735
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\f scans (Fair, 1990)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular prism'
_exptl_crystal_F_000             900
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .10
_refine_diff_density_max         .64
_refine_diff_density_min         -.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3633
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          .062
_refine_ls_R_factor_gt           .050
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.104P)^2^+0.576P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .155
_reflns_number_gt                3007
_reflns_number_total             3633
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    bm1424.cif
_[local]_cod_data_source_block   I
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_cod_original_cell_volume        2070.4(7)
_cod_database_code               2011403
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Zn -.38984(5) .38958(2) .75272(3) .0461(2) Uani d . 1 . . Zn
Ca -.5000 .5000 .5000 .0421(3) Uani d S 1 . . Ca
O11 -.3384(4) .54016(17) .6467(2) .0713(9) Uani d . 1 . . O
O12 -.2845(4) .47508(15) .7904(2) .0637(8) Uani d . 1 . . O
O21 -.3621(5) .39771(17) .4998(3) .0767(10) Uani d . 1 A . O
O22 -.3158(5) .33211(18) .6426(2) .0832(11) Uani d . 1 A . O
O31 -.6418(4) .4493(2) .6244(3) .0800(10) Uani d . 1 . . O
O32 -.6130(4) .38731(18) .7680(3) .0694(9) Uani d . 1 . . O
N -.3063(4) .32705(16) .8818(2) .0502(8) Uani d . 1 . . N
C11 -.2756(5) .5307(2) .7375(3) .0544(10) Uani d . 1 . . C
C12 -.1815(8) .5877(3) .7923(5) .097(2) Uani d . 1 . . C
H12A -.2487 .6276 .7965 .117 Uiso calc R 1 . . H
H12B -.1002 .6003 .7473 .117 Uiso calc R 1 . . H
C13 -.1063(10) .5727(4) .9032(6) .131(3) Uani d . 1 . . C
H13A -.0482 .6124 .9302 .197 Uiso calc R 1 . . H
H13B -.0371 .5340 .9005 .197 Uiso calc R 1 . . H
H13C -.1853 .5621 .9499 .197 Uiso calc R 1 . . H
C21 -.3087(7) .3469(3) .5444(3) .0760(16) Uani d . 1 . . C
C22 -.2821(14) .2835(6) .4709(9) .078(3) Uiso d PD .50 A 1 C
C23 -.127(2) .2523(13) .4947(19) .171(9) Uiso d PD .50 A 1 C
C22A -.1881(13) .3042(5) .4809(9) .070(2) Uiso d PD .50 A 1 C
C23A -.203(2) .2299(7) .5095(13) .109(5) Uiso d PD .50 A 1 C
C31 -.6963(5) .4200(2) .6981(4) .0565(10) Uani d . 1 . . C
C32 -.8689(7) .4237(5) .7058(6) .107(2) Uani d D 1 . . C
C33 -.952(2) .4576(9) .6095(14) .127(5) Uiso d P .50 . . C
C33A -.935(2) .3804(9) .7896(14) .140(6) Uiso d PD .50 . . C
C41 -.2489(6) .2659(2) .8581(4) .0678(13) Uani d . 1 . . C
H41A -.2472 .2542 .7859 .081 Uiso calc R 1 . . H
C42 -.1912(8) .2182(3) .9359(4) .0886(18) Uani d . 1 . . C
H42A -.1515 .1760 .9158 .106 Uiso calc R 1 . . H
C43 -.1939(8) .2344(3) 1.0408(4) .0866(18) Uani d . 1 . . C
H43A -.1564 .2030 1.0935 .104 Uiso calc R 1 . . H
C44 -.2529(6) .2983(2) 1.0708(3) .0603(11) Uani d . 1 . . C
C45 -.2600(7) .3176(3) 1.1790(4) .0820(16) Uani d . 1 . . C
H45A -.2209 .2881 1.2340 .098 Uiso calc R 1 . . H
C46 -.3235(8) .3789(3) 1.2035(4) .0889(18) Uani d . 1 . . C
H46A -.3301 .3908 1.2752 .107 Uiso calc R 1 . . H
C47 -.3792(7) .4244(3) 1.1217(4) .0803(16) Uani d . 1 . . C
H47A -.4213 .4667 1.1393 .096 Uiso calc R 1 . . H
C48 -.3725(6) .4073(2) 1.0168(3) .0610(11) Uani d . 1 . . C
H48A -.4098 .4382 .9632 .073 Uiso calc R 1 . . H
C49 -.3106(5) .3444(2) .9881(3) .0481(9) Uani d . 1 . . C
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Zn .0684(3) .0363(3) .0331(3) .00394(19) .0020(2) .00242(16)
Ca .0562(6) .0370(5) .0319(5) .0036(4) -.0022(4) .0060(4)
O11 .097(2) .0605(19) .0512(18) -.0162(17) -.0215(16) .0100(15)
O12 .091(2) .0450(16) .0518(17) -.0092(15) -.0097(14) .0068(13)
O21 .111(3) .063(2) .0559(19) .0370(19) .0087(18) .0084(15)
O22 .143(3) .071(2) .0371(16) .044(2) .0173(18) .0032(15)
O31 .077(2) .095(3) .070(2) -.0065(19) .0180(17) .0270(19)
O32 .075(2) .075(2) .0580(19) .0005(16) .0060(16) .0168(16)
N .076(2) .0386(17) .0350(15) .0095(15) .0018(14) .0041(13)
C11 .070(3) .044(2) .047(2) -.0069(19) -.0065(18) .0047(18)
C12 .128(5) .067(3) .088(4) -.038(3) -.036(4) .011(3)
C13 .164(7) .111(6) .103(5) -.037(5) -.065(5) -.011(4)
C21 .126(4) .065(3) .038(2) .044(3) .012(2) .004(2)
C31 .062(3) .053(2) .055(2) -.008(2) .011(2) -.009(2)
C32 .061(3) .146(7) .117(5) -.013(4) .025(3) .016(5)
C41 .114(4) .042(2) .046(2) .021(2) .000(2) -.0029(18)
C42 .154(5) .048(3) .061(3) .036(3) -.002(3) .003(2)
C43 .149(5) .051(3) .057(3) .032(3) -.005(3) .018(2)
C44 .085(3) .053(2) .041(2) .008(2) -.001(2) .0094(18)
C45 .125(5) .081(4) .037(2) .023(3) -.002(2) .016(2)
C46 .140(5) .088(4) .039(3) .016(4) .013(3) -.002(2)
C47 .125(5) .068(3) .047(3) .027(3) .006(3) -.007(2)
C48 .091(3) .051(2) .041(2) .016(2) .005(2) .0049(19)
C49 .067(2) .042(2) .0351(19) .0024(17) .0035(16) .0037(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca .2262 .3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 Zn O22 . . 119.41(17) yes
O12 Zn O32 . . 116.19(15) yes
O22 Zn O32 . . 117.04(17) yes
O12 Zn N . . 101.05(13) yes
O22 Zn N . . 95.84(13) yes
O32 Zn N . . 100.44(14) yes
O11 Ca O21 . . 91.10(13) yes
O11 Ca O31 . . 85.87(13) yes
O21 Ca O31 . . 86.64(14) yes
O31 Ca O21 . 3_466 93.36(14) ?
O31 Ca O11 3_466 . 94.13(13) ?
O31 Ca O21 3_466 . 93.36(14) ?
O21 Ca O11 3_466 . 88.90(13) ?
O31 Ca O11 . 3_466 94.13(13) ?
O21 Ca O11 . 3_466 88.90(13) ?
C11 O11 Ca . . 149.1(3) no
C11 O12 Zn . . 130.8(3) no
C21 O21 Ca . . 151.2(3) no
C21 O22 Zn . . 127.6(3) no
C31 O31 Ca . . 170.5(3) no
C31 O32 Zn . . 115.2(3) no
C41 N C49 . . 118.7(3) no
C41 N Zn . . 117.0(3) no
C49 N Zn . . 124.3(2) no
O11 C11 O12 . . 124.5(4) no
O11 C11 C12 . . 119.1(4) no
O12 C11 C12 . . 116.4(4) no
C11 C12 C13 . . 116.5(5) no
O21 C21 O22 . . 125.6(4) no
O21 C21 C22 . . 116.3(5) no
O22 C21 C22 . . 114.4(6) no
O21 C21 C22A . . 115.7(5) no
O22 C21 C22A . . 117.2(5) no
C22 C21 C22A . . 33.1(5) no
C23 C22 C21 . . 112.7(13) no
C23A C22A C21 . . 107.7(9) no
O31 C31 O32 . . 122.0(4) no
O31 C31 C32 . . 119.0(5) no
O32 C31 C32 . . 119.1(5) no
C33 C32 C33A . . 128.4(12) no
C33 C32 C31 . . 111.9(8) no
C33A C32 C31 . . 117.8(10) no
N C41 C42 . . 123.4(4) no
C43 C42 C41 . . 118.9(4) no
C42 C43 C44 . . 120.3(4) no
C43 C44 C45 . . 122.7(4) no
C43 C44 C49 . . 118.2(4) no
C45 C44 C49 . . 119.1(4) no
C46 C45 C44 . . 120.3(4) no
C45 C46 C47 . . 120.4(5) no
C48 C47 C46 . . 120.5(5) no
C47 C48 C49 . . 121.0(4) no
N C49 C48 . . 120.7(3) no
N C49 C44 . . 120.6(4) no
C48 C49 C44 . . 118.7(4) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn O12 . 1.924(3) yes
Zn O22 . 1.924(3) yes
Zn O32 . 1.951(3) yes
Zn N . 2.086(3) yes
Ca O11 . 2.323(3) yes
Ca O21 . 2.310(3) yes
Ca O31 . 2.287(3) no
Ca O11 3_466 2.323(3) no
Ca O21 3_466 2.310(3) no
Ca O31 3_466 2.287(3) no
O11 C11 . 1.220(5) no
O12 C11 . 1.270(5) no
O21 C21 . 1.199(5) no
O22 C21 . 1.265(5) no
O31 C31 . 1.213(5) no
O32 C31 . 1.246(5) no
N C41 . 1.327(5) no
N C49 . 1.372(5) no
C11 C12 . 1.494(6) no
C12 C13 . 1.497(8) no
C21 C22 . 1.563(12) no
C21 C22A . 1.597(11) no
C22 C23 . 1.472(16) no
C22A C23A . 1.492(14) no
C31 C32 . 1.501(7) no
C32 C33 . 1.490(19) no
C32 C33A . 1.498(15) no
C41 C42 . 1.396(6) no
C42 C43 . 1.347(7) no
C43 C44 . 1.403(7) no
C44 C45 . 1.408(6) no
C44 C49 . 1.417(5) no
C45 C46 . 1.355(8) no
C46 C47 . 1.397(7) no
C47 C48 . 1.357(6) no