A second monoclinic polymorph of {bis[5-methyl-3-(trifluoromethyl)pyrazol-1-yl]borato}{tris[5-methyl-3-(trifluoromethyl)pyrazol-1-yl]borato}cobalt(II): a structure containing a B—H···Co agostic interaction
Stibrany, Robert T.; Potenza, Joseph A.; Acta Crystallographica Section E 67 (2011) m911–m912; doi:10.1107/S1600536811021994

data_2230844
_publ_contact_author
;
 Robert T. Stibrany
 Department of Chemistry and Chemical Biology
 Rutgers, The State University of New Jersey
 610 Taylor Road
 Piscataway, New Jersey 08854 USA
;
_publ_section_title
;
 A second monoclinic polymorph of
 {bis[5-methyl-3-(trifluoromethyl)pyrazol-1-yl]borato}{tris[5-methyl-3-(trifluoromethyl)pyrazol-1-yl]borato}cobalt(II):
 a structure containing a B---H&#x00B7;&#x00B7;&#x00B7;Co agostic
 interaction
;
_journal_coeditor_code           RZ2601
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m911
_journal_page_last               m912
_journal_paper_doi               10.1107/S1600536811021994
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co (C10 H10 B F6 N4) (C15 H13 B F9 N6)]'
_chemical_formula_moiety         'C25 H23 B2 Co F15 N10'
_chemical_formula_sum            'C25 H23 B2 Co F15 N10'
_chemical_formula_weight         829.08
_chemical_name_systematic
{Bis[5-methyl-3-(trifluoromethyl)pyrazol-1-yl]borato}{tris[5-methyl-3-(trifluoromethyl)pyrazol-1-yl]borato}cobalt(II)
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 102.721(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.593(2)
_cell_length_b                   12.1167(13)
_cell_length_c                   30.720(3)
_cell_measurement_reflns_used    910
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.40
_cell_measurement_theta_min      2.21
_cell_volume                     6750.9(12)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2000)'
_computing_data_collection       'SMART WNT/2000 (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2000)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and ORTEP32 (Farrugia, 1997)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            32390
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+6.3500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                5522
_reflns_number_total             7431
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2601.cif
_cod_data_source_block           I
_cod_original_cell_volume        6751.1(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2230844
_cod_database_fobs_code          2230844