Transition-metal imido-boroxide complexes: a structural and spectroscopic investigation of the influence of boron
Cole, Sarah C.; Coles, Martyn P.; Hitchcock, Peter B.; Journal of the Chemical Society, Dalton Transactions  (2002) 4168–; doi:10.1039/b207277g

data_7012060
_publ_section_title
;
 Transition-metal imido-boroxide complexes: a structural and
 spectroscopic investigation of the influence of boron
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4168
_journal_paper_doi               10.1039/b207277g
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H78 B2 Mo N2 O2'
_chemical_formula_sum            'C60 H78 B2 Mo N2 O2'
_chemical_formula_weight         976.8
_chemical_name_common            '[Mo(OBMes2)2(NC6H3iPr2)2]'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-02-22T09:04:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.2134(4)
_cell_length_b                   19.0999(5)
_cell_length_c                   44.5065(13)
_cell_measurement_reflns_used    51265
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     11232.3(6)
_computing_cell_refinement       'HKL Scalepack'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1566
_diffrn_reflns_av_unetI/netI     0.1782
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            48346
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.51
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.98
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1223
_refine_ls_number_reflns         12794
_refine_ls_number_restraints     721
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1613
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                6842
_reflns_number_total             12794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207277g.txt
_cod_data_source_block           (2)feb1102
_cod_original_sg_symbol_H-M      Pbc2(1)
_cod_database_code               7012060