On the remarkable structural diversity and kinetic lability of TpC*CaX complexes (X = NSi2Me6, OC6H4-p-Me, TpC*) where TpC* = tris[3-(2-methoxy-1,1-dimethylethyl)pyrazolyl]hydroborate.
Chisholm, Malcolm H; Gallucci, Judith C; Yaman, Gülşah; Young, Tanya; Chemical communications (Cambridge, England) 34 (2009) 1828–1830; doi:10.1039/b818375a

data_7104292
_publ_section_title
;
 On the remarkable structural diversity and kinetic lability of TpC*CaX
 complexes (X = NSi2Me6, OC6H4-p-Me, TpC*) where TpC* =
 tris[3-(2-methoxy-1,1-dimethylethyl)pyrazolyl]hydroborate.
;
_journal_issue                   14
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1828
_journal_page_last               1830
_journal_paper_doi               10.1039/b818375a
_journal_volume                  34
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H40 B1 N6 O3, C24 H40 B1 Ca1 N6 O3'
_chemical_formula_sum            'C48 H80 B2 Ca N12 O6'
_chemical_formula_weight         982.94
_chemical_name_common            'Chisholm 1492a'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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      2.3
_audit_creation_date             2008-09-30T17:41:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.840(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2546(2)
_cell_length_b                   16.7217(3)
_cell_length_c                   24.6146(5)
_cell_measurement_reflns_used    7697
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      22.465
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     5720.45(17)
_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      230(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.340732E-1
_diffrn_orient_matrix_UB_12      -0.503023E-1
_diffrn_orient_matrix_UB_13      -0.62267E-2
_diffrn_orient_matrix_UB_21      0.530064E-1
_diffrn_orient_matrix_UB_22      0.323423E-1
_diffrn_orient_matrix_UB_23      -0.96708E-2
_diffrn_orient_matrix_UB_31      0.347339E-1
_diffrn_orient_matrix_UB_32      -0.111E-4
_diffrn_orient_matrix_UB_33      0.400493E-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  0.085
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51480
_diffrn_reflns_theta_full        22.45
_diffrn_reflns_theta_max         22.45
_diffrn_reflns_theta_min         2.09
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular rod'
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         7420
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0971P)^2^+19.3301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2301
_refine_ls_wR_factor_ref         0.2589
_reflns_number_gt                4516
_reflns_number_total             7420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818375a.txt
_cod_data_source_block           Chisholm1492a
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7104292