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_7012063
_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         'C52 H65 N3 O2 Ti1'
_chemical_formula_sum            'C52 H65 N3 O2 Ti'
_chemical_formula_weight         811.97
_chemical_name_common            '[Ti(py)2(NtBu)(OCHMes2)2]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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             2002-06-14T14:45:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                82.370(1)
_cell_angle_beta                 89.957(1)
_cell_angle_gamma                83.821(1)
_cell_formula_units_Z            4
_cell_length_a                   10.5789(1)
_cell_length_b                   19.5500(3)
_cell_length_c                   22.5063(3)
_cell_measurement_reflns_used    55867
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4586.25(10)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  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  0.0707
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60894
_diffrn_reflns_theta_full        24.76
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.9965
_exptl_absorpt_correction_T_min  0.9111
_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    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         15458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0429P)^2^+5.6436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1476
_reflns_number_gt                11334
_reflns_number_total             15458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207277g.txt
_cod_data_source_block           (5)jun1102
_cod_original_cell_volume        4586.3(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012063