Tetraethylammonium dicarbonyl(dicyanomethylene)[tris(3,5-dimethyl-1-pyrazolyl)hydroborato]molybdenum(0)
Ferguson, George; Lalor, Fergus J.; O'Neill, S. A.; Acta Crystallographica Section E 59 (2003) m644–m646; doi:10.1107/S1600536803015794

data_2202337
_publ_section_title
;Tetraethylammonium
 dicarbonyl(dicyanomethylene)[tris(3,5-dimethyl-1-pyrazolyl)hydroborato]molybdenum(0)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m644
_journal_page_last               m646
_journal_paper_doi               10.1107/S1600536803015794
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'(C8 H20 N) [Mo (C15 H22 B N6) (C3 N2) (C1 O1)2]'
_chemical_formula_moiety         'C8 H20 N 1+, C20 H22 B Mo N8 O2 1-'
_chemical_formula_sum            'C28 H42 B Mo N9 O2'
_chemical_formula_weight         643.46
_chemical_name_systematic
;
Tetraethylammonium dicarbonyl(dicyanomethylene)[tris(3,5-dimethyl-1-
pyrazolyl)hydroborato]molybdenum(0)
;
_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     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 109.989(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.153(3)
_cell_length_b                   8.113(2)
_cell_length_c                   20.161(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      15.20
_cell_measurement_theta_min      9.60
_cell_volume                     6172.0(19)
_computing_cell_refinement       'SET4 and CELDIM in CAD-4-PC Software'
_computing_data_collection       'CAD-4-PC Software (Enraf-Nonius, 1992)'
_computing_data_reduction        'DATRD2 in NRCVAX96 (Gabe et al., 1989)'
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'NRCVAX96 via Patterson heavy-atom method'
_diffrn_ambient_temperature      294.0(10)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.013
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6846
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_correction_T_min  0.8910
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.417
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0458P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                4379
_reflns_number_total             6761
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6306.cif
_cod_data_source_block           1
_cod_original_cell_volume        6172.0(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202337
_cod_database_fobs_code          2202337