Tetracarbonyl(trifluoromethyl)cobalt(I) [Co(CO)4(CF3)] as a Precursor to New Cobalt Trifluoromethyl and Difluorocarbene Complexes
Harrison, Daniel J.; Daniels, Alex L.; Korobkov, Ilia; Baker, R. Tom; Organometallics 34 (2015) 4598–; doi:10.1021/acs.organomet.5b00674

data_4086286
_publ_section_title
;
 Tetracarbonyl(trifluoromethyl)cobalt(I) [Co(CO)4(CF3)] as a Precursor to
 New Cobalt Trifluoromethyl and Difluorocarbene Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4598
_journal_paper_doi               10.1021/acs.organomet.5b00674
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C32.5 H28 Co F3 O2 P2'
_chemical_formula_weight         628.42
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 96.6240(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8852(3)
_cell_length_b                   12.0588(2)
_cell_length_c                   15.3725(3)
_cell_measurement_reflns_used    9324
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.43
_cell_volume                     2925.04(9)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.993
_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  0.0188
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29290
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.327
_diffrn_reflns_theta_min         2.126
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         7244
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+1.0835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6449
_reflns_number_total             7244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00674_si_003.cif
_cod_data_source_block           tb163a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_formula_sum        'C32.50 H28 Co F3 O2 P2'
_cod_database_code               4086286
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.936
_shelxl_version_number           2013-4
_shelx_res_checksum              20430
_shelx_hkl_checksum              67275