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_7021650
_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         'C16 H20 Co F12 N4 O2 P2'
_chemical_formula_sum            'C16 H20 Co F12 N4 O2 P2'
_chemical_formula_weight         649.23
_chemical_name_common
;bis(trimethylphosphine-oxide)-bis(3,5-
bis(trifluoromethyl)pyrazolate)cobalt(ii)
;
_chemical_name_systematic
;
bis(trimethylphosphine-oxide)-bis(3,5-bis(trifluoromethyl)pyrazolate)cobalt(ii)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.582(3)
_cell_angle_beta                 104.265(4)
_cell_angle_gamma                101.473(4)
_cell_formula_units_Z            2
_cell_length_a                   10.1321(13)
_cell_length_b                   10.2434(13)
_cell_length_c                   13.9848(17)
_cell_measurement_reflns_used    9159
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      3.09
_cell_volume                     1342.6(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku SCX-Mini with Mercury CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4713
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.523
_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    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4713
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0852
_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^)+(0.0562P)^2^+4.2924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2183
_reflns_number_gt                3468
_reflns_number_total             4713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50758k.txt
_cod_data_source_block           CoOPME3Pz2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7021650