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_4089290
_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            'C35.5 H28.5 Br Co N3.5 O4.5'
_chemical_formula_weight         714.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.6059(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0405(5)
_cell_length_b                   8.5418(3)
_cell_length_c                   24.4517(9)
_cell_measurement_reflns_used    5965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.38
_cell_volume                     2929.49(18)
_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  0.0752
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            45652
_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         30.508
_diffrn_reflns_theta_min         1.641
_exptl_absorpt_coefficient_mu    2.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.027
_exptl_transmission_factor_max   0.914
_exptl_transmission_factor_min   0.780
_refine_diff_density_max         0.534
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0494P)^2^+2.2206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5995
_reflns_number_total             8948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00186_si_001.cif
_cod_data_source_block           dm2dc2_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 2/n'
_cod_original_formula_sum        'C35.50 H28.50 Br Co N3.50 O4.50'
_cod_database_code               4089290
_shelx_estimated_absorpt_t_min   0.744
_shelx_estimated_absorpt_t_max   0.948
_shelxl_version_number           2013-4
_shelx_res_checksum              37614
_shelx_hkl_checksum              10480