Molybdenum Complexes ofC,C-Bis(ethynyl)carboranes: Design, Synthesis, and Study of a Weakly Coupled Mixed-Valence Compound
Brown, Neil J.; Lancashire, Hannah N.; Fox, Mark A.; Collison, David; Edge, Ruth; Yufit, Dmitry S.; Howard, Judith A. K.; Whiteley, Mark W.; Low, Paul J.; Organometallics 30 (2011) 884–; doi:10.1021/om1010353

data_4063923
_publ_section_title
;
 Molybdenum Complexes ofC,C-Bis(ethynyl)carboranes: Design, Synthesis, and
 Study of a Weakly Coupled Mixed-Valence Compound
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              884
_journal_paper_doi               10.1021/om1010353
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C37 H42 B10 Mo P2'
_chemical_formula_sum            'C37 H42 B10 Mo P2'
_chemical_formula_weight         752.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 109.278(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3792(3)
_cell_length_b                   18.2803(4)
_cell_length_c                   15.8979(3)
_cell_measurement_reflns_used    6927
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.32
_cell_measurement_theta_min      2.23
_cell_volume                     3670.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46711
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         9744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                7409
_reflns_number_total             9744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1010353_si_002.cif
_cod_data_source_block           1_09SRV198
_cod_original_cell_volume        3670.22(21)
_cod_database_code               4063923