#------------------------------------------------------------------------------
#$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $
#$Revision: 91933 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/04/2010438.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_2010438
loop_
_publ_author_name
'Huhmann, Jean L.'
'Corey, Joyce Y.'
'Rath, Nigam P.'
_publ_section_title
;
 (Tetraphenylporphyrinato)zirconium(IV) Diacetate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              195
_journal_page_last               197
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C49 H36 Cl2 N4 O4 Zr1'
_chemical_formula_sum            'C49 H36 Cl2 N4 O4 Zr'
_chemical_formula_weight         906.9
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.
_cell_angle_beta                 104.23(4)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   17.985(7)
_cell_length_b                   15.900(7)
_cell_length_c                   15.042(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      9
_cell_volume                     4169(3)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       \q-2\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6492
_diffrn_reflns_theta_max         25.0
_diffrn_standards_decay_%        <4
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.6809
_exptl_absorpt_correction_T_min  0.6480
_exptl_absorpt_correction_type   'empirical, \y-scan'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       needle
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.72
_refine_ls_goodness_of_fit_obs   1.07
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3689
_refine_ls_R_factor_obs          0.0763
_refine_ls_shift/esd_max         0.2
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'w = 1/[\s^2^(F) + 0.0022F^2^]'
_refine_ls_wR_factor_obs         0.0822
_reflns_number_observed          2191
_reflns_number_total             3689
_reflns_observed_criterion       F>3\s(F)
_[local]_cod_data_source_file    bk1042.cif
_[local]_cod_data_source_block   bk1042_structure_1_of_1
_[local]_cod_cif_authors_sg_H-M  'C 2/c'
_[local]_cod_chemical_formula_sum_orig 'C49 H36 Cl2 N4 O4 Zr1'
_cod_original_cell_volume        4172(2)
_cod_database_code               2010438
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,-y,1/2+z
-x,-y,-z
-x,y,1/2-z
1/2+x,1/2+y,z
1/2+x,1/2-y,1/2+z
1/2-x,1/2-y,-z
1/2-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Zr .0 .31010(10) .2500 .0290(10)
O(1) .0411(3) .2111(3) .1671(4) .047(2)
O(2) .1035(3) .2268(4) .3087(4) .046(2)
N(1) -.0508(4) .3714(4) .1141(4) .035(2)
N(2) .1007(4) .3792(4) .2181(4) .035(2)
C(1) -.1293(5) .3822(5) .0764(5) .035(3)
C(2) -.1421(5) .3808(6) -.0215(6) .045(3)
C(3) -.0757(5) .3704(5) -.0444(6) .046(3)
C(4) -.0169(5) .3675(5) .0415(5) .036(3)
C(5) .0613(5) .3692(5) .0487(5) .036(3)
C(6) .1160(5) .3827(5) .1332(5) .037(3)
C(7) .1942(5) .4045(6) .1414(6) .046(4)
C(8) .2276(5) .4136(6) .2306(6) .042(3)
C(9) .1705(5) .3961(5) .2803(5) .038(3)
C(10) .1835(5) .3965(5) .3736(5) .035(3)
C(11) .2646(5) .4135(6) .4293(5) .040(3)
C(12) .3148(6) .3480(7) .4533(7) .068(4)
C(13) .3895(5) .3655(9) .5047(8) .075(5)
C(14) .4113(6) .4428(10) .5317(7) .081(5)
C(15) .3611(6) .5094(8) .5083(7) .071(5)
C(16) .2876(5) .4935(7) .4559(6) .057(4)
C(17) .0913(5) .3579(6) -.0349(6) .041(3)
C(18) .0741(5) .4135(6) -.1077(6) .048(4)
C(19) .1021(6) .4009(7) -.1849(6) .057(4)
C(20) .1472(6) .3331(9) -.1892(7) .071(5)
C(21) .1659(6) .2778(8) -.1170(8) .075(5)
C(22) .1382(5) .2898(6) -.0401(7) .062(4)
C(23) .0952(5) .1877(6) .2344(7) .048(3)
C(24) .1471(6) .1173(7) .2272(8) .085(5)
C(25) .0 .8234(19) .2500 .175(11)
Cl .0478(8) .9169(10) .2176(10) .224(6)
Cl' .0433(6) .8531(8) .1762(7) .161(4)
H(2A) -.1914 .3860 -.0639 .080
H(3A) -.0678 .3662 -.1050 .080
H(7A) .2185 .4108 .0916 .080
H(8A) .2799 .4295 .2570 .080
H(12A) .2992 .2916 .4348 .080
H(13A) .4258 .3204 .5211 .080
H(14A) .4626 .4526 .5676 .080
H(15A) .3767 .5652 .5290 .080
H(16A) .2523 .5392 .4372 .080
H(18A) .0423 .4613 -.1043 .080
H(19A) .0897 .4398 -.2351 .080
H(20A) .1659 .3241 -.2431 .080
H(21A) .1983 .2304 -.1201 .080
H(22A) .1513 .2516 .0108 .080
H(24A) .1846 .1356 .1957 .080
H(24B) .1726 .0984 .2876 .080
H(24C) .1177 .0719 .1938 .080
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr O(1) . . 2.243(6) yes
Zr N(1) . . 2.246(6) yes
Zr C(23) . . 2.640(10) yes
Zr O(2) . . 2.278(6) yes
Zr N(2) . . 2.268(7) yes
O(1) C(23) . . 1.274(10) yes
N(1) C(1) . . 1.397(10) yes
N(2) C(6) . . 1.372(11) yes
C(1) C(2) . . 1.434(12) yes
C(3) C(4) . . 1.456(11) yes
C(5) C(6) . . 1.418(10) yes
C(7) C(8) . . 1.337(11) yes
C(9) C(10) . . 1.365(11) yes
O(2) C(23) . . 1.254(11) yes
N(1) C(4) . . 1.377(12) yes
N(2) C(9) . . 1.395(9) yes
C(2) C(3) . . 1.330(14) yes
C(4) C(5) . . 1.385(12) yes
C(6) C(7) . . 1.424(12) yes
C(8) C(9) . . 1.438(13) yes
C(23) C(24) . . 1.480(15) yes
C(1) C(10A) . . 1.389(13) no
C(10) C(11) . . 1.517(10) no
C(11) C(16) . . 1.367(13) no
C(13) C(14) . . 1.32(2) no
C(15) C(16) . . 1.385(13) no
C(17) C(22) . . 1.387(14) no
C(19) C(20) . . 1.361(17) no
C(21) C(22) . . 1.381(17) no
C(25) Cl . . 1.84(3) no
C(5) C(17) . . 1.496(13) no
C(11) C(12) . . 1.367(13) no
C(12) C(13) . . 1.404(14) no
C(14) C(15) . . 1.380(18) no
C(17) C(18) . . 1.381(12) no
C(18) C(19) . . 1.390(14) no
C(20) C(21) . . 1.374(16) no
C(25) Cl' . . 1.577(15) no
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(1) Zr O(2) 57.2(2) yes
O(1) Zr O(2A) 74.1(2) yes
O(1) Zr O(1A) 90.9(3) yes
O(2) Zr O(2A) 108.9(3) yes
N(1) Zr N(2) 76.4(2) yes
O(1) Zr N(1) 85.1(2) yes
O(1) Zr N(2) 80.4(2) yes
O(2A) Zr N(1) 77.8(2) yes
O(2) Zr N(2) 75.2(2) yes
N(2) Zr N(1A) 79.3(2) yes
N(2) Zr N(2A) 122.1(3) yes
C(23) Zr C(23A) 85.1(4) yes
(2) Zr N(1) 135.7(2) no
O(1) Zr C(23) 28.8(2) no
N(1) Zr C(23) 111.5(3) no
N(2) Zr O(1A) 147.9(2) no
N(2) Zr O(2A) 144.9(2) no
N(1) Zr N(1A) 128.6(3) no
C(23) Zr N(1A) 105.8(3) no
C(23) Zr N(2A) 160.9(3) no
O(2) Zr C(23A) 91.4(2) no
N(2) Zr C(23A) 16.9(3) no
Zr O(1) C(23) 93.2(6) no
Zr N(1) C(1) 124.6(5) no
C(1) N(1) C(4) 106.5(6) no
Zr N(2) C(9) 125.8(5) no
N(1) C(1) C(2) 107.8(8) no
C(2) C(1) C(10A) 127.1(7) no
C(2) C(3) C(4) 106.1(8) no
N(1) C(4) C(5) 125.2(7) no
C(4) C(5) C(6) 122.7(8) no
C(6) C(5) C(17) 117.3(7) no
N(2) C(6) C(7) 110.5(7) no
C(6) C(7) C(8) 107.6(8) no
N(2) C(9) C(8) 109.2(7) no
C(8) C(9) C(10) 124.7(7) no
C(9) C(10) C(1A) 126.2(7) no
C(10) C(11) C(12) 119.5(8) no
C(12) C(11) C(16) 120.0(8) no
C(12) C(13) C(14) 121.7(11) no
C(14) C(15) C(16) 118.6(11) no
C(5) C(17) C(18) 122.2(8) no
C(18) C(17) C(22) 118.4(9) no
C(18) C(19) C(20) 119.8(9) no
C(20) C(21) C(22) 120.4(11) no
Zr C(23) O(1) 58.0(5) no
O(1) C(23) O(2) 117.6(8) no
O(1) C(23) C(24) 122.3(9) no
Cl C(25) Cl' 39.5(8) no
O(2) Zr C(23) 28.3(2) no
N(2) Zr C(23) 76.6(3) no
N(1) Zr O(1A) 134.0(2) no
C(23) Zr O(1A) 80.9(3) no
C(23) Zr O(2A) 91.4(2) no
O(1) Zr C(23A) 80.9(3) no
N(1) Zr C(23A) 105.8(3) no
Zr O(2) C(23) 92.1(5) no
Zr N(1) C(4) 122.8(5) no
Zr N(2) C(6) 124.8(5) no
C(6) N(2) C(9) 105.3(7) no
N(1) C(1) C(10A) 125.0(7) no
C(1) C(2) C(3) 109.9(7) no
N(1) C(4) C(3) 109.6(7) no
C(3) C(4) C(5) 124.9(8) no
C(4) C(5) C(17) 120.0(7) no
N(2) C(6) C(5) 125.1(8) no
C(5) C(6) C(7) 124.4(8) no
C(7) C(8) C(9) 107.4(7) no
N(2) C(9) C(10) 126.1(8) no
C(9) C(10) C(11) 117.8(8) no
C(11) C(10) C(1A) 116.0(7) no
C(10) C(11) C(16) 120.6(8) no
C(11) C(12) C(13) 118.3(10) no
C(13) C(14) C(15) 120.5(10) no
C(11) C(16) C(15) 120.9(9) no
C(5) C(17) C(22) 119.4(8) no
C(17) C(18) C(19) 120.9(9) no
C(19) C(20) C(21) 120.1(11) no
C(17) C(22) C(21) 120.3(9) no
Zr C(23) O(2) 59.6(5) no
Zr C(23) C(24) 178.1(8) no
O(2) C(23) C(24) 120.1(8) no
Cl C(25) Cl'A 106.7(17) no
_journal_paper_doi 10.1107/S0108270194008553