Alkyl chlorido hydridotris(3,5-dimethylpyrazolyl)borate imido niobium and tantalum(v) complexes: synthesis, conformational states of alkyl groups in solid and solution, X-ray diffraction and multinuclear magnetic resonance spectroscopy studies.
Galájov, Miguel; García, Carlos; Gómez, Manuel; Gómez-Sal, Pilar; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5747–5758; doi:10.1039/c3dt53353k

data_7029393
_publ_section_title
;
 Alkyl chlorido hydridotris(3,5-dimethylpyrazolyl)borate imido niobium and
 tantalum(v) complexes: synthesis, conformational states of alkyl groups
 in solid and solution, X-ray diffraction and multinuclear magnetic
 resonance spectroscopy studies.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5747
_journal_page_last               5758
_journal_paper_doi               10.1039/c3dt53353k
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C23 H42 B1 Cl1 N7 Nb1 Si1),0.5(C6 H14)'
_chemical_formula_sum            'C49 H91 B2 Cl2 N14 Nb2 Si2'
_chemical_formula_weight         1210.88
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
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_audit_creation_date             2013-11-07T13:58:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.009(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9978(7)
_cell_length_b                   38.529(5)
_cell_length_c                   17.280(2)
_cell_measurement_reflns_used    261
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16.25
_cell_measurement_theta_min      3.48
_cell_measurement_wavelength     0.71073
_cell_volume                     6591.4(12)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Giacovazzo et al, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1379
_diffrn_reflns_av_unetI/netI     0.1897
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41498
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        26.8
_diffrn_reflns_theta_max         26.8
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.22
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         13770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1781
_refine_ls_R_factor_gt           0.071
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1897
_reflns_number_gt                6528
_reflns_number_total             13770
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt53353k.txt
_cod_data_source_block           4a
_cod_original_cell_volume        6591.5(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7029393