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_4086288
_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            'C36 H33 Co F3 O P3'
_chemical_formula_weight         690.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9032(5)
_cell_length_b                   19.0147(14)
_cell_length_c                   21.3182(14)
_cell_measurement_reflns_used    5513
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.35
_cell_volume                     3203.6(4)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26231
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_min         2.142
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
; 
 Flack x determined using 2179 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.014(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.759
_reflns_friedel_fraction_full    0.991
_reflns_friedel_fraction_max     0.968
_reflns_number_gt                6163
_reflns_number_total             7908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00674_si_004.cif
_cod_data_source_block           tb175
_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_database_code               4086288
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.821
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              73761
_shelx_hkl_checksum              59089