Aromatic interactions in hydrotris(3-methylindazolyl)borate organoniobium complexes: control of an alkyne ligand orientation in the crystal
Pascal Oulié; Johannes Teichert; Laure Vendier; Céline Dablemont; Michel Etienne; New Journal of Chemistry 30 (2006) 679–; doi:10.1039/b601652a

data_7052261
_publ_section_title
;
 Aromatic interactions in hydrotris(3-methylindazolyl)borate
 organoniobium complexes: control of an alkyne ligand orientation in
 the crystal
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              679
_journal_paper_doi               10.1039/b601652a
_journal_volume                  30
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H30 B Cl2 N6 Nb'
_chemical_formula_sum            'C33 H30 B Cl2 N6 Nb'
_chemical_formula_weight         685.25
_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
_cell_angle_alpha                90
_cell_angle_beta                 109.858(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1301(14)
_cell_length_b                   19.875(2)
_cell_length_c                   16.4137(16)
_cell_measurement_reflns_used    3320
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.2783
_cell_measurement_theta_min      2.6892
_cell_measurement_wavelength     0.71073
_cell_volume                     3415.0(7)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_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      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_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  0.0779
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25314
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         3.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.54
_exptl_absorpt_correction_T_max  0.9150
_exptl_absorpt_correction_T_min  0.8812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                3929
_reflns_number_total             6958
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b601652a.txt
_cod_data_source_block           compound
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7052261