Synthesis and structures of Co bis-trifluoromethylpyrazolate complexes.
Rivers, Joseph H.; Jones, Richard A.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 12898–12907; doi:10.1039/c3dt50758k

data_7021647
_publ_section_title
;
 Synthesis and structures of Co bis-trifluoromethylpyrazolate complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12898
_journal_page_last               12907
_journal_paper_doi               10.1039/c3dt50758k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C18 H12 Co F18 N6 P, C12 H38 Co P4'
_chemical_formula_sum            'C30 H50 Co2 F18 N6 P5'
_chemical_formula_weight         1109.47
_chemical_name_common
;
(dihydrido-tetrakis(trimethylphosphine)-cobalt(iii))(tris-bis-
3,5-(trifluorometh
;
_chemical_name_systematic
;
[dihydrido-tetrakis(trimethylphosphine)-cobalt(iii)][tris-bis-3,5-(trifluoromethyl)pyrazolate-trimethylphosphine-cobalt(ii)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.308(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.0753(2)
_cell_length_b                   68.7275(12)
_cell_length_c                   13.7230(9)
_cell_measurement_reflns_used    54652
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.32
_cell_measurement_theta_min      6.58
_cell_volume                     9502.4(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;
SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-Axis Spider '
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_av_sigmaI/netI    0.1156
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       78
_diffrn_reflns_limit_k_min       -83
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            152403
_diffrn_reflns_theta_full        69.99
_diffrn_reflns_theta_max         69.99
_diffrn_reflns_theta_min         6.58
_exptl_absorpt_coefficient_mu    7.992
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_T_min  0.255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001).
The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4504
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.294
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1201
_refine_ls_number_reflns         17894
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.1697
_refine_ls_R_factor_gt           0.1018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+2.3266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                10569
_reflns_number_total             17894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50758k.txt
_cod_data_source_block           Co2P5Pz3H2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7021647