#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:08:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179881 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/77/7017739.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_7017739
loop_
_publ_author_name
'Mujkic, Monika'
'Lentz, Dieter'
_publ_section_title
;
 Syntheses of highly unsaturated isocyanides via organometallic pathways.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              839
_journal_page_last               849
_journal_paper_doi               10.1039/c1dt11382h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C32 Co4 Cr2 F4 N2 O22'
_chemical_formula_weight         1180.06
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.994(3)
_cell_length_b                   11.837(3)
_cell_length_c                   24.944(6)
_cell_measurement_reflns_used    960
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     4131.9(17)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'SMART (Bruker-AXS)'
_computing_data_reduction        'SAINT (Bruker-AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS ASMART CCD'
_diffrn_measurement_method       'omega scan'
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32362
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.564
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0666
_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)+(0.0413P)²+46.0795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                3152
_reflns_number_total             3671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11382h.txt
_cod_data_source_block           1monika
_cod_original_cell_volume        4131.9(16)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7017739
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
Co1 Co 0.60533(7) 0.15626(8) 0.53666(4) 0.0285(3) Uani 1 1 d
Co2 Co 0.51324(8) 0.18593(8) 0.45337(4) 0.0302(3) Uani 1 1 d
Cr3 Cr 0.54155(12) 0.45359(12) 0.71005(5) 0.0446(4) Uani 1 1 d
F2 F 0.3030(3) 0.1332(4) 0.5367(2) 0.0495(13) Uani 1 1 d
C3 C 0.4697(5) 0.1528(6) 0.5265(3) 0.0300(16) Uani 1 1 d
O7 O 0.6387(5) 0.3986(5) 0.5576(2) 0.0465(15) Uani 1 1 d
N1 N 0.4454(5) 0.3033(5) 0.6236(3) 0.0392(16) Uani 1 1 d
C2 C 0.3835(6) 0.1809(6) 0.5567(3) 0.0291(16) Uani 1 1 d
O11 O 0.5429(6) 0.4316(6) 0.4410(3) 0.073(2) Uani 1 1 d
O1 O 0.6164(7) 0.6148(7) 0.7943(3) 0.081(3) Uani 1 1 d
O2 O 0.4471(6) 0.3126(7) 0.7963(3) 0.076(2) Uani 1 1 d
C4 C 0.5070(5) 0.0594(6) 0.5033(3) 0.0275(15) Uani 1 1 d
O9 O 0.3270(4) 0.1635(6) 0.4012(3) 0.0509(16) Uani 1 1 d
O4 O 0.6546(6) 0.5932(6) 0.6299(3) 0.066(2) Uani 1 1 d
O8 O 0.7886(4) 0.0866(5) 0.4902(3) 0.0514(16) Uani 1 1 d
C10O C 0.3988(6) 0.1737(7) 0.4213(3) 0.0368(18) Uani 1 1 d
F1 F 0.2880(4) 0.2623(5) 0.6194(2) 0.0567(14) Uani 1 1 d
C4O C 0.6109(8) 0.5402(8) 0.6585(4) 0.051(2) Uani 1 1 d
C11O C 0.5914(6) 0.1240(8) 0.4027(4) 0.041(2) Uani 1 1 d
O6 O 0.6106(6) 0.0720(6) 0.6470(3) 0.063(2) Uani 1 1 d
C9O C 0.7193(6) 0.1112(6) 0.5082(3) 0.0335(17) Uani 1 1 d
O10 O 0.6358(5) 0.0780(7) 0.3726(3) 0.071(2) Uani 1 1 d
C12O C 0.5312(7) 0.3380(7) 0.4456(3) 0.045(2) Uani 1 1 d
C7O C 0.6110(6) 0.1032(7) 0.6048(4) 0.043(2) Uani 1 1 d
C6O C 0.4827(7) 0.3590(7) 0.6561(3) 0.041(2) Uani 1 1 d
C1 C 0.3744(6) 0.2470(7) 0.5988(3) 0.0368(18) Uani 1 1 d
C8O C 0.6283(6) 0.3055(7) 0.5500(3) 0.0375(18) Uani 1 1 d
C5O C 0.6495(9) 0.3560(9) 0.7151(4) 0.059(3) Uani 1 1 d
C3O C 0.4347(10) 0.5503(11) 0.7049(5) 0.076(3) Uani 1 1 d
O5 O 0.7133(7) 0.2989(8) 0.7186(4) 0.098(3) Uani 1 1 d
C2O C 0.4800(8) 0.3661(8) 0.7638(4) 0.054(2) Uani 1 1 d
C1O C 0.5897(9) 0.5523(8) 0.7640(4) 0.059(3) Uani 1 1 d
O3 O 0.3717(8) 0.6090(10) 0.6981(5) 0.119(4) Uani 1 1 d
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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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_site_symmetry_1
_geom_angle_site_symmetry_3
C7O Co1 C9O 103.0(4) . .
C7O Co1 C8O 99.1(4) . .
C9O Co1 C8O 101.5(4) . .
C7O Co1 C3 99.2(4) . .
C9O Co1 C3 143.9(3) . .
C8O Co1 C3 102.6(3) . .
C7O Co1 C4 103.0(3) . .
C9O Co1 C4 105.9(3) . .
C8O Co1 C4 139.5(3) . .
C3 Co1 C4 40.7(3) . .
C7O Co1 Co2 149.4(3) . .
C9O Co1 Co2 99.8(3) . .
C8O Co1 Co2 96.1(3) . .
C3 Co1 Co2 51.3(2) . .
C4 Co1 Co2 50.5(2) . .
C10O Co2 C11O 101.1(4) . .
C10O Co2 C12O 98.9(4) . .
C11O Co2 C12O 103.9(4) . .
C10O Co2 C4 100.5(3) . .
C11O Co2 C4 99.2(4) . .
C12O Co2 C4 146.1(3) . .
C10O Co2 C3 97.0(3) . .
C11O Co2 C3 138.6(4) . .
C12O Co2 C3 109.7(4) . .
C4 Co2 C3 40.5(3) . .
C10O Co2 Co1 145.9(3) . .
C11O Co2 Co1 102.3(3) . .
C12O Co2 Co1 99.0(3) . .
C4 Co2 Co1 51.5(2) . .
C3 Co2 Co1 49.6(2) . .
C3O Cr3 C2O 91.2(6) . .
C3O Cr3 C1O 87.5(5) . .
C2O Cr3 C1O 89.8(4) . .
C3O Cr3 C5O 179.9(6) . .
C2O Cr3 C5O 89.0(5) . .
C1O Cr3 C5O 92.6(5) . .
C3O Cr3 C4O 91.7(5) . .
C2O Cr3 C4O 176.3(5) . .
C1O Cr3 C4O 88.1(4) . .
C5O Cr3 C4O 88.1(4) . .
C3O Cr3 C6O 88.1(5) . .
C2O Cr3 C6O 89.0(4) . .
C1O Cr3 C6O 175.4(5) . .
C5O Cr3 C6O 91.9(4) . .
C4O Cr3 C6O 93.3(4) . .
C4 C3 C2 136.5(7) . .
C4 C3 Co1 72.0(5) . .
C2 C3 Co1 138.2(6) . .
C4 C3 Co2 69.2(4) . .
C2 C3 Co2 133.7(5) . .
Co1 C3 Co2 79.1(3) . .
C6O N1 C1 158.1(8) . .
C1 C2 F2 117.4(7) . .
C1 C2 C3 128.9(8) . .
F2 C2 C3 113.7(6) . .
C3 C4 C4 143.2(9) . 5_656
C3 C4 Co2 70.3(4) . .
C4 C4 Co2 133.5(8) 5_656 .
C3 C4 Co1 67.3(4) . .
C4 C4 Co1 135.7(7) 5_656 .
Co2 C4 Co1 78.0(3) . .
O9 C10O Co2 178.4(7) . .
O4 C4O Cr3 176.8(9) . .
O10 C11O Co2 174.4(8) . .
O8 C9O Co1 178.1(7) . .
O11 C12O Co2 179.5(9) . .
O6 C7O Co1 177.0(9) . .
N1 C6O Cr3 178.5(8) . .
C2 C1 F1 118.6(8) . .
C2 C1 N1 126.1(8) . .
F1 C1 N1 115.3(7) . .
O7 C8O Co1 177.2(8) . .
O5 C5O Cr3 179.3(12) . .
O3 C3O Cr3 175.4(13) . .
O2 C2O Cr3 177.2(11) . .
O1 C1O Cr3 176.6(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 C7O 1.813(10) .
Co1 C9O 1.826(9) .
Co1 C8O 1.826(8) .
Co1 C3 1.915(8) .
Co1 C4 1.975(7) .
Co1 Co2 2.4699(15) .
Co2 C10O 1.796(9) .
Co2 C11O 1.826(10) .
Co2 C12O 1.828(8) .
Co2 C4 1.950(7) .
Co2 C3 1.963(7) .
Cr3 C3O 1.888(13) .
Cr3 C2O 1.901(10) .
Cr3 C1O 1.905(10) .
Cr3 C5O 1.906(12) .
Cr3 C4O 1.911(10) .
Cr3 C6O 1.936(9) .
F2 C2 1.356(9) .
C3 C4 1.353(11) .
C3 C2 1.460(10) .
O7 C8O 1.128(10) .
N1 C6O 1.168(11) .
N1 C1 1.347(11) .
C2 C1 1.315(11) .
O11 C12O 1.125(10) .
O1 C1O 1.121(11) .
O2 C2O 1.127(11) .
C4 C4 1.429(14) 5_656
O9 C10O 1.129(10) .
O4 C4O 1.129(11) .
O8 C9O 1.107(10) .
F1 C1 1.327(9) .
C11O O10 1.115(11) .
O6 C7O 1.116(11) .
C5O O5 1.124(13) .
C3O O3 1.134(14) .
