Reactions of [Mo(CBr)(CO)2{HB(pzMe2)3}] (pz = pyrazol-1-yl) with Amines: Synthesis of Amino, Pyridinium, and Thiolato Carbyne Complexes
Cordiner, Richard L.; Hill, Anthony F.; Wagler, Jörg; Organometallics 27 (2008) 4532–; doi:10.1021/om8004756

data_4071928
_publ_section_title
;
 Reactions of [Mo(&#xE5FC;CBr)(CO)2{HB(pzMe2)3}] (pz = pyrazol-1-yl) with
 Amines: Synthesis of Amino, Pyridinium, and Thiolato Carbyne Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4532
_journal_paper_doi               10.1021/om8004756
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C25 H32 B Mo N8 O2, 4(C H Cl3), Br'
_chemical_formula_sum            'C29 H36 B Br Cl12 Mo N8 O2'
_chemical_formula_weight         1140.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 93.7520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9825(3)
_cell_length_b                   15.8754(3)
_cell_length_c                   19.5854(4)
_cell_measurement_reflns_used    245424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.631
_cell_measurement_theta_min      2.546
_cell_volume                     4648.46(16)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Scalepack
_computing_molecular_graphics    'ORTEP32 for windows (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            120026
_diffrn_reflns_theta_full        33.00
_diffrn_reflns_theta_max         33.00
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.869
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.342
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         34623
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+2.6941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                27597
_reflns_number_total             34623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8004756_si_004.cif
_cod_data_source_block           rc01501_p21
_cod_original_sg_symbol_Hall     P2yb
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4071928