Pyrazolate-bridging dinucleating ligands containing hydrogen-bond donors: synthesis and structure of their cobalt analogues.
Zinn, Paul J.; Powell, Douglas R.; Day, Victor W.; Hendrich, Michael P.; Sorrell, Thomas N.; Borovik, A. S.; Inorganic chemistry 45 (2006) 3484–3486; doi:10.1021/ic060009n

data_4350208
_publ_section_title
;
 Pyrazolate-bridging dinucleating ligands containing hydrogen-bond donors:
 synthesis and structure of their cobalt analogues.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3484
_journal_page_last               3486
_journal_paper_doi               10.1021/ic060009n
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C55 H113.5 Cl Co2 N14.5 O4.5'
_chemical_formula_weight         1203.41
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.9450(10)
_cell_angle_beta                 98.9220(10)
_cell_angle_gamma                94.2240(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6311(6)
_cell_length_b                   15.3318(7)
_cell_length_c                   17.3877(8)
_cell_measurement_reflns_used    8747
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      2.224
_cell_volume                     3343.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39968
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.9118
_exptl_absorpt_correction_T_min  0.8573
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Purple/wine
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rhombus
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         19262
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0380
_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/[\s^2^(Fo^2^)+(0.0663P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                15074
_reflns_number_total             19262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060009nrom20060102_055313.cif
_cod_data_source_block           k24a
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C55 H113.50 Cl Co2 N14.50 O4.50'
_cod_database_code               4350208