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_4350209
_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            'C61 H126 Cl Co2 N15 O5'
_chemical_formula_weight         1303.08
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.132(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.293(3)
_cell_length_b                   22.333(4)
_cell_length_c                   21.971(4)
_cell_measurement_reflns_used    7738
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.79
_cell_measurement_theta_min      2.13
_cell_volume                     7409(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0910
_diffrn_reflns_av_sigmaI/netI    0.2062
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            88982
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.5975
_exptl_absorpt_correction_T_min  0.5563
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Purple/wine
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.752
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1573
_refine_ls_number_reflns         42956
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.765
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                18819
_reflns_number_total             42956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060009nrom20060102_055313.cif
_cod_data_source_block           k28a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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 

 Corrected the value of the '_refine_diff_density_rms' data item
 by removing an ASCII start of heading (SOH) symbol.

 Antanas Vaitkus,
 2019-12-11
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4350209