[1,2-Bis(diphenylphosphino)ethane]{2-[bis(diphenylphosphinomethyl)amino]pyridinium}fluoridohydrazidatomolybdenum(IV) bis(tetrafluoridoborate)
Stephan, Gerald; Näther, Christian; Tuczek, Felix; Acta Crystallographica Section E 64 (2008) m629–; doi:10.1107/S1600536808008635

data_2218058
_publ_section_title
;[1,2-Bis(diphenylphosphino)ethane]{2-[bis(diphenylphosphinomethyl)amino]pyridinium}fluoridohydrazidatomolybdenum(IV)
 bis(tetrafluoridoborate)
;
_journal_coeditor_code           BT2688
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m629
_journal_paper_doi               10.1107/S1600536808008635
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'[Mo F (N2 H2) (C31 H29 N2 P2) (C26 H24 P2)] (B F4)2'
_chemical_formula_moiety         'C57 H55 F Mo N4 P4, 2(B F4)'
_chemical_formula_sum            'C57 H55 B2 F9 Mo N4 P4'
_chemical_formula_weight         1208.49
_chemical_name_systematic
;[1,2-Bis(diphenylphosphino)ethane]{2-
[bis(diphenylphosphinomethyl)amino]pyridinium}fluoridohydrazidatomolybdenum(IV)
bis(tetrafluoridoborate)
;
_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                 94.438(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5791(6)
_cell_length_b                   31.2199(16)
_cell_length_c                   13.8330(9)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      10
_cell_volume                     5416.2(5)
_computing_cell_refinement       'IPDS program package'
_computing_data_collection       'IPDS program package (Stoe & Cie, 1998b)'
_computing_data_reduction        'IPDS program package'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'CIFTAB in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       \f
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24176
_diffrn_reflns_theta_full        24.10
_diffrn_reflns_theta_max         24.10
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1998a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.537
_refine_ls_extinction_coef       0.0045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         8538
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0748P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                6783
_reflns_number_total             8538
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2688.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2218058
_cod_database_fobs_code          2218058