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_7012059
_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         'C44 H62 B2 Mo N2 O2'
_chemical_formula_sum            'C44 H62 B2 Mo N2 O2'
_chemical_formula_weight         768.52
_chemical_name_common            '[Zn{N(SiMe3)2}{MesNPPh2CHPPh2NMes}]'
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      41
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_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             2002-03-22T14:19:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0505(6)
_cell_length_b                   27.3517(7)
_cell_length_c                   8.4738(2)
_cell_measurement_reflns_used    10905
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4415.4(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.86479E-1
_diffrn_orient_matrix_UB_12      0.242136E-1
_diffrn_orient_matrix_UB_13      0.81954E-2
_diffrn_orient_matrix_UB_21      -0.767717E-1
_diffrn_orient_matrix_UB_22      0.273907E-1
_diffrn_orient_matrix_UB_23      -0.65379E-2
_diffrn_orient_matrix_UB_31      -0.235379E-1
_diffrn_orient_matrix_UB_32      -0.3765E-3
_diffrn_orient_matrix_UB_33      0.514345E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.047
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14970
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         3.92
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.8449
_exptl_absorpt_correction_T_min  0.7779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    'riding; torsion refined for o-methyls'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3706
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+8.4475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0909
_reflns_number_gt                2900
_reflns_number_total             3706
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207277g.txt
_cod_data_source_block           (1)mar1402
_cod_original_sg_symbol_H-M      Aba2
_cod_database_code               7012059