Synthesis and Characterization of Alkoxycarbonyl Cobalt Complexes via Direct Carbonylation Methods
Chambers, Dana R.; Sullivan, Raymond E.; Martin, David B. C.; Organometallics 36 (2017) 1630–; doi:10.1021/acs.organomet.7b00186

data_4089289
_publ_section_title
;
 Synthesis and Characterization of Alkoxycarbonyl Cobalt Complexes via
 Direct Carbonylation Methods
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1630
_journal_paper_doi               10.1021/acs.organomet.7b00186
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C30 H27 Co N2 O5'
_chemical_formula_weight         554.46
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.5084(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7197(8)
_cell_length_b                   11.1312(7)
_cell_length_c                   17.5704(11)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.87
_cell_measurement_theta_min      2.17
_cell_volume                     2486.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker 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  0.0413
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56934
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         1.602
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.509
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.063
_exptl_transmission_factor_max   0.928
_exptl_transmission_factor_min   0.776
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7268
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+2.9256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6410
_reflns_number_total             7268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00186_si_001.cif
_cod_data_source_block           dm1dc1_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4089289
_shelx_estimated_absorpt_t_min   0.706
_shelx_estimated_absorpt_t_max   0.955
_shelxl_version_number           2013-4
_shelx_res_checksum              17267
_shelx_hkl_checksum              24327