#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006318.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_2006318
loop_
_publ_author_name
'Fl\"orke, U.'
'Haupt, H.-J.'
_publ_section_title
;
 \m-Bromo-\m-cyclohexylphosphido-bis(tetracarbonylmanganese) and
 \m-Bromo-\m-(pentacarbonylmanganese)phosphido-bis(tetracarbonylmanganese)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              876
_journal_page_last               879
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Mn3 Br P H (CO)13]'
_chemical_formula_sum            'C13 H Br Mn3 O13 P'
_chemical_formula_weight         640.84
_chemical_name_systematic
;
 \m-bromo-\m-(pentacarbonylmanganese)phosphido-bis(tetracarbonylmanganese)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                81.57(2)
_cell_angle_beta                 84.59(2)
_cell_angle_gamma                74.68(2)
_cell_formula_units_Z            2
_cell_length_a                   8.735(2)
_cell_length_b                   8.9530(10)
_cell_length_c                   13.837(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      7
_cell_volume                     1030.6(4)
_computing_structure_refinement  'SHELXTL (Siemens, 1995)'
_computing_structure_solution    'SHELXTL (Siemens, 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4984
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        insignificant
_diffrn_standards_interval_count 400
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    3.889
_exptl_absorpt_correction_T_max  0.652
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   '\y scans'
_exptl_absorpt_process_details   'North, Phillips & Mathews (1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_description       prism
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.696
_refine_ls_extinction_coef       0.0037(6)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_obs          0.0398
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.2887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.0951
_refine_ls_wR_factor_obs         0.0861
_reflns_number_observed          3612
_reflns_number_total             4760
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    ka1213.cif
_[local]_cod_data_source_block   II
_cod_database_code               2006318
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Br1 0.0359(2) 0.0420(2) 0.0486(2) -0.0001(2) -0.0131(2) -0.0091(2)
Mn1 0.0309(3) 0.0326(3) 0.0310(3) -0.0073(2) -0.0035(2) -0.0060(2)
Mn2 0.0323(3) 0.0281(3) 0.0378(3) -0.0033(2) -0.0016(2) -0.0064(2)
Mn3 0.0309(3) 0.0370(3) 0.0338(3) -0.0028(2) -0.0068(2) -0.0063(2)
P1 0.0282(5) 0.0282(4) 0.0298(5) -0.0049(4) -0.0034(3) -0.0035(4)
C1 0.043(2) 0.056(3) 0.039(2) -0.017(2) -0.007(2) -0.004(2)
O1 0.071(2) 0.105(3) 0.054(2) -0.047(2) -0.002(2) 0.019(2)
C2 0.042(2) 0.049(2) 0.035(2) -0.009(2) -0.005(2) -0.013(2)
O2 0.049(2) 0.060(2) 0.065(2) 0.014(2) -0.010(2) -0.025(2)
C3 0.039(2) 0.043(2) 0.047(2) -0.008(2) -0.005(2) -0.004(2)
O3 0.069(2) 0.069(2) 0.063(2) -0.027(2) 0.004(2) 0.013(2)
C4 0.044(2) 0.039(2) 0.043(2) -0.011(2) -0.004(2) -0.006(2)
O4 0.073(2) 0.064(2) 0.065(2) -0.025(2) -0.026(2) -0.018(2)
C5 0.047(2) 0.040(2) 0.047(2) -0.011(2) -0.001(2) -0.009(2)
O5 0.076(2) 0.072(2) 0.062(2) -0.027(2) -0.011(2) -0.028(2)
C6 0.042(2) 0.046(2) 0.044(2) -0.007(2) -0.004(2) -0.008(2)
O6 0.081(3) 0.084(3) 0.067(2) -0.036(2) 0.005(2) 0.013(2)
C7 0.047(2) 0.032(2) 0.055(3) -0.005(2) -0.005(2) -0.002(2)
O7 0.073(2) 0.054(2) 0.088(3) -0.020(2) 0.002(2) 0.017(2)
C8 0.049(2) 0.041(2) 0.052(2) -0.005(2) -0.001(2) -0.011(2)
O8 0.054(2) 0.051(2) 0.106(3) 0.014(2) 0.010(2) -0.015(2)
C9 0.038(2) 0.041(2) 0.049(2) -0.006(2) -0.008(2) -0.011(2)
O9 0.060(2) 0.080(2) 0.060(2) -0.020(2) 0.016(2) -0.024(2)
C10 0.040(2) 0.044(2) 0.039(2) 0.000(2) -0.011(2) 0.001(2)
O10 0.072(2) 0.045(2) 0.074(2) -0.023(2) -0.017(2) 0.008(2)
C11 0.038(2) 0.053(3) 0.050(2) -0.009(2) -0.005(2) -0.019(2)
O11 0.075(3) 0.066(2) 0.103(3) -0.035(2) 0.004(2) -0.030(2)
C12 0.048(2) 0.048(2) 0.035(2) -0.001(2) -0.015(2) -0.001(2)
O12 0.069(2) 0.084(3) 0.039(2) 0.002(2) 0.006(2) -0.008(2)
C13 0.044(2) 0.052(3) 0.048(2) -0.002(2) -0.011(2) -0.013(2)
O13 0.058(2) 0.083(3) 0.071(2) 0.010(2) -0.033(2) -0.010(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_thermal_displace_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_type_symbol
Br1 -0.49418(5) 1.46353(5) 0.64243(3) 0.04300(10) Uani d 1 Br
Mn1 -0.25693(6) 1.23252(6) 0.61989(4) 0.03130(10) Uani d 1 Mn
Mn2 -0.36874(6) 1.56354(6) 0.77028(4) 0.0333(2) Uani d 1 Mn
Mn3 0.06511(6) 1.21783(6) 0.83829(4) 0.0345(2) Uani d 1 Mn
P1 -0.14311(10) 1.35790(10) 0.72709(6) 0.0291(2) Uani d 1 P
C1 -0.1738(5) 1.3552(5) 0.5191(3) 0.0448(9) Uani d 1 C
O1 -0.1244(4) 1.4289(5) 0.4578(2) 0.0750(10) Uani d 1 O
C2 -0.0835(5) 1.0731(5) 0.6129(3) 0.0413(9) Uani d 1 C
O2 0.0285(4) 0.9716(4) 0.6100(2) 0.0612(9) Uani d 1 O
C3 -0.3455(5) 1.1209(5) 0.7242(3) 0.0436(9) Uani d 1 C
O3 -0.4006(4) 1.0500(4) 0.7857(2) 0.0680(9) Uani d 1 O
C4 -0.3571(5) 1.1646(5) 0.5297(3) 0.0419(9) Uani d 1 C
O4 -0.4142(4) 1.1234(4) 0.4716(2) 0.0634(9) Uani d 1 O
C5 -0.2704(5) 1.6227(5) 0.8599(3) 0.0443(9) Uani d 1 C
O5 -0.2046(4) 1.6571(4) 0.9177(2) 0.0659(9) Uani d 1 O
C6 -0.4445(5) 1.4258(5) 0.8640(3) 0.0443(9) Uani d 1 C
O6 -0.4946(5) 1.3451(5) 0.9218(3) 0.0770(10) Uani d 1 O
C7 -0.2862(5) 1.6883(5) 0.6710(3) 0.0460(10) Uani d 1 C
O7 -0.2348(4) 1.7655(4) 0.6108(3) 0.0740(10) Uani d 1 O
C8 -0.5488(5) 1.7198(5) 0.7847(3) 0.0480(10) Uani d 1 C
O8 -0.6606(4) 1.8183(4) 0.7938(3) 0.0760(10) Uani d 1 O
C9 0.1917(5) 1.1810(5) 0.7232(3) 0.0427(9) Uani d 1 C
O9 0.2661(4) 1.1630(4) 0.6532(3) 0.0659(9) Uani d 1 O
C10 -0.0014(5) 1.0370(5) 0.8378(3) 0.0431(9) Uani d 1 C
O10 -0.0442(4) 0.9275(4) 0.8388(2) 0.0628(9) Uani d 1 O
C11 0.1151(5) 1.4092(5) 0.8289(3) 0.0460(10) Uani d 1 C
O11 0.1456(4) 1.5255(4) 0.8216(3) 0.0760(10) Uani d 1 O
C12 -0.0774(5) 1.2693(5) 0.9440(3) 0.0450(10) Uani d 1 C
O12 -0.1661(4) 1.2989(4) 1.0074(2) 0.0690(10) Uani d 1 O
C13 0.2287(5) 1.1111(5) 0.9178(3) 0.0490(10) Uani d 1 C
O13 0.3248(4) 1.0457(4) 0.9675(3) 0.0740(10) Uani d 1 O
H1 -0.052(4) 1.438(4) 0.665(3) 0.040(10) Uiso d 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
Mn1 Br1 Mn2 94.48(3) y
C2 Mn1 C4 92.6(2) n
C2 Mn1 C3 91.2(2) n
C4 Mn1 C3 92.2(2) n
C2 Mn1 C1 91.7(2) n
C4 Mn1 C1 89.7(2) n
C3 Mn1 C1 176.5(2) n
C2 Mn1 P1 93.83(13) n
C4 Mn1 P1 171.90(13) n
C3 Mn1 P1 92.50(13) n
C1 Mn1 P1 85.29(13) n
C2 Mn1 Br1 175.23(12) n
C4 Mn1 Br1 92.03(13) n
C3 Mn1 Br1 87.60(13) n
C1 Mn1 Br1 89.42(13) n
P1 Mn1 Br1 81.62(3) y
C5 Mn2 C8 92.8(2) n
C5 Mn2 C6 91.4(2) n
C8 Mn2 C6 92.2(2) n
C5 Mn2 C7 91.2(2) n
C8 Mn2 C7 91.3(2) n
C6 Mn2 C7 175.5(2) n
C5 Mn2 P1 94.86(13) n
C8 Mn2 P1 171.49(14) n
C6 Mn2 P1 91.19(13) n
C7 Mn2 P1 84.96(13) n
C5 Mn2 Br1 176.32(13) n
C8 Mn2 Br1 90.80(14) n
C6 Mn2 Br1 87.89(13) n
C7 Mn2 Br1 89.28(14) n
P1 Mn2 Br1 81.55(3) y
C13 Mn3 C12 93.0(2) n
C13 Mn3 C10 91.3(2) n
C12 Mn3 C10 90.0(2) n
C13 Mn3 C11 94.9(2) n
C12 Mn3 C11 90.3(2) n
C10 Mn3 C11 173.7(2) n
C13 Mn3 C9 93.2(2) n
C12 Mn3 C9 173.7(2) n
C10 Mn3 C9 90.9(2) n
C11 Mn3 C9 88.1(2) n
C13 Mn3 P1 177.57(13) n
C12 Mn3 P1 89.36(12) n
C10 Mn3 P1 89.09(12) n
C11 Mn3 P1 84.66(13) n
C9 Mn3 P1 84.43(13) n
Mn1 P1 Mn2 101.64(4) y
Mn1 P1 Mn3 123.66(4) y
Mn2 P1 Mn3 124.11(4) y
O1 C1 Mn1 179.5(4) n
O2 C2 Mn1 178.7(3) n
O3 C3 Mn1 177.7(4) n
O4 C4 Mn1 177.4(4) n
O5 C5 Mn2 178.3(4) n
O6 C6 Mn2 178.0(4) n
O7 C7 Mn2 179.2(4) n
O8 C8 Mn2 179.5(4) n
O9 C9 Mn3 178.1(4) n
O10 C10 Mn3 178.7(4) n
O11 C11 Mn3 178.9(4) n
O12 C12 Mn3 178.4(4) n
O13 C13 Mn3 178.3(4) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Mn1 2.5439(9) y
Br1 Mn2 2.5457(9) y
Mn1 C2 1.792(4) y
Mn1 C4 1.845(4) y
Mn1 C3 1.859(4) y
Mn1 C1 1.860(4) y
Mn1 P1 2.4092(11) y
Mn2 C5 1.786(4) y
Mn2 C8 1.825(4) y
Mn2 C6 1.855(5) y
Mn2 C7 1.855(4) y
Mn2 P1 2.4113(12) y
Mn3 C13 1.853(4) n
Mn3 C12 1.858(4) n
Mn3 C10 1.860(4) n
Mn3 C11 1.861(5) n
Mn3 C9 1.870(4) n
Mn3 P1 2.4505(12) y
C1 O1 1.122(5) n
C2 O2 1.148(5) n
C3 O3 1.134(5) n
C4 O4 1.136(5) n
C5 O5 1.147(5) n
C6 O6 1.133(5) n
C7 O7 1.140(5) n
C8 O8 1.141(5) n
C9 O9 1.121(5) n
C10 O10 1.135(5) n
C11 O11 1.129(5) n
C12 O12 1.127(5) n
C13 O13 1.118(5) n