Modulating the Primary and Secondary Coordination Spheres within a Series of Co(II)-OH Complexes.
Jones, Jason R.; Ziller, Joseph W.; Borovik, A. S.; Inorganic chemistry 56 (2017) 1112–1120; doi:10.1021/acs.inorgchem.6b01956

data_4345042
_publ_section_title
;
 Modulating the Primary and Secondary Coordination Spheres within a Series
 of Co(II)-OH Complexes.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1112
_journal_page_last               1120
_journal_paper_doi               10.1021/acs.inorgchem.6b01956
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C81 H102 Co3 K6 N12 O21 S9'
_chemical_formula_weight         2279.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 111.2036(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4569(14)
_cell_length_b                   32.796(2)
_cell_length_c                   18.3948(13)
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      2.18
_cell_volume                     10943.2(13)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            113990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.709
_diffrn_reflns_theta_min         1.446
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  0.8012
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             4716
_exptl_crystal_size_max          0.673
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.159
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     1242
_refine_ls_number_reflns         20819
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+72.1580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2025
_refine_ls_wR_factor_ref         0.2138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17114
_reflns_number_total             20819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01956_si_003.cif
_cod_data_source_block           asb414
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4345041--4345042.cif.
;
_cod_original_cell_volume        10943.1(13)
_cod_database_code               4345042
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.578
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              51533
_shelx_hkl_checksum              8124
_shelx_fab_checksum              47295