#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:06:01 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178490 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/01/4060176.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4060176
_journal_name_full               Organometallics
_journal_year                    2005
_chemical_formula_sum            'C32 H22 Co4 Fe O14'
_chemical_formula_weight         922.07
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3936(3)
_cell_length_b                   10.4536(2)
_cell_length_c                   26.6811(5)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     3456.74(12)
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 9109
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_theta_max         20.62
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         1753
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0689P)²+0.9471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                1603
_reflns_number_total             1753
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4060176
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.90568(4) 0.17874(6) 0.60316(2) 0.0256(3) Uani 1 1 d . . .
Co2 Co 1.09741(5) 0.20591(6) 0.58095(2) 0.0242(3) Uani 1 1 d . . .
Fe1 Fe 1.0000 0.01228(8) 0.7500 0.0208(3) Uani 1 2 d S . .
O1 O 0.9419(3) 0.4132(3) 0.70162(12) 0.0514(10) Uani 1 1 d D . .
H1 H 0.980(4) 0.358(4) 0.7240(15) 0.062 Uiso 1 1 d D . .
C1 C 1.0101(3) 0.4207(4) 0.65759(14) 0.0303(11) Uani 1 1 d . . .
C2 C 1.0155(3) 0.2899(4) 0.63457(14) 0.0231(11) Uani 1 1 d . . .
C3 C 1.0321(3) 0.1671(4) 0.64749(14) 0.0231(10) Uani 1 1 d . . .
C4 C 1.0726(3) 0.0803(4) 0.68561(14) 0.0230(11) Uani 1 1 d . . .
C5 C 1.1337(4) 0.1135(4) 0.72933(14) 0.0248(11) Uani 1 1 d . . .
H5 H 1.1504 0.1981 0.7398 0.030 Uiso 1 1 calc R . .
C6 C 1.1648(4) 0.0010(4) 0.75411(16) 0.0280(12) Uani 1 1 d . . .
H6 H 1.2066 -0.0038 0.7839 0.034 Uiso 1 1 calc R . .
C7 C 1.1230(4) -0.1041(4) 0.72700(16) 0.0302(11) Uani 1 1 d . . .
H7 H 1.1314 -0.1918 0.7355 0.036 Uiso 1 1 calc R . .
C8 C 1.0663(4) -0.0558(4) 0.68485(15) 0.0259(11) Uani 1 1 d . . .
H8 H 1.0301 -0.1058 0.6603 0.031 Uiso 1 1 calc R . .
C9 C 0.9578(5) 0.5172(5) 0.6228(2) 0.0478(14) Uani 1 1 d . . .
H9A H 0.8839 0.4901 0.6152 0.072 Uiso 1 1 calc R . .
H9B H 0.9994 0.5226 0.5916 0.072 Uiso 1 1 calc R . .
H9C H 0.9563 0.6013 0.6390 0.072 Uiso 1 1 calc R . .
C10 C 1.1216(4) 0.4648(4) 0.67316(17) 0.0350(12) Uani 1 1 d . . .
H10A H 1.1546 0.4002 0.6949 0.052 Uiso 1 1 calc R . .
H10B H 1.1159 0.5459 0.6914 0.052 Uiso 1 1 calc R . .
H10C H 1.1664 0.4768 0.6433 0.052 Uiso 1 1 calc R . .
O101 O 0.7288(3) 0.2389(3) 0.67208(12) 0.0462(9) Uani 1 1 d . . .
C101 C 0.7973(4) 0.2147(5) 0.64553(17) 0.0339(12) Uani 1 1 d . . .
O102 O 0.8289(3) 0.3197(3) 0.51386(13) 0.0474(10) Uani 1 1 d . . .
C102 C 0.8564(4) 0.2653(5) 0.54832(18) 0.0332(11) Uani 1 1 d . . .
O103 O 0.8694(3) -0.0943(4) 0.58103(13) 0.0562(10) Uani 1 1 d . . .
C103 C 0.8822(4) 0.0114(6) 0.58889(17) 0.0351(12) Uani 1 1 d . . .
O201 O 1.0968(3) 0.3883(4) 0.49614(15) 0.0642(13) Uani 1 1 d . . .
C201 C 1.0949(4) 0.3187(5) 0.5287(2) 0.0353(13) Uani 1 1 d . . .
O202 O 1.3207(3) 0.2416(3) 0.61342(12) 0.0457(9) Uani 1 1 d . . .
C202 C 1.2344(4) 0.2281(4) 0.60085(15) 0.0301(11) Uani 1 1 d . . .
O203 O 1.1243(3) -0.0464(4) 0.53407(14) 0.0583(10) Uani 1 1 d . . .
C203 C 1.1145(4) 0.0507(5) 0.55132(17) 0.0335(12) Uani 1 1 d . . .
