Reactivity of a Series of Isostructural Cobalt Pincer Complexes with CO2, CO, and H(+)
Shaffer, David W.; Johnson, Samantha I.; Rheingold, Arnold L.; Ziller, Joseph W.; Goddard, 3rd, William A; Nielsen, Robert J.; Yang, Jenny Y.; Inorganic chemistry  (2014) 141203160549001–; doi:10.1021/ic5021725

data_4341827
_publ_section_title
;
 Reactivity of a Series of Isostructural Cobalt Pincer Complexes with CO2,
 CO, and H(+)
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141203160549001
_journal_paper_doi               10.1021/ic5021725
_journal_year                    2014
_chemical_formula_sum            'C23 H44 B Co F4 N4 P2'
_chemical_formula_weight         584.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.299(2)
_cell_length_b                   21.997(3)
_cell_length_c                   32.508(4)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.50
_cell_volume                     11655(3)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2013.10-0, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (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 0.999
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            131283
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.253
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.9007
_exptl_absorpt_correction_T_min  0.7763
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/2'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4928
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.283
_refine_diff_density_max         2.334
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         13202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+28.8128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10167
_reflns_number_total             13202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5021725_si_006.cif
_cod_data_source_block           jyy9
_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 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4341827
_shelx_estimated_absorpt_t_min   0.757
_shelx_estimated_absorpt_t_max   0.817
_shelxl_version_number           2014-3
_shelx_res_checksum              54740
_shelx_hkl_checksum              13646