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_7104290
_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         'C30 H58 B Ca N7 O3 Si2'
_chemical_formula_sum            'C30 H58 B Ca N7 O3 Si2'
_chemical_formula_weight         671.9
_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             2008-10-01T14:39:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.351(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1496(5)
_cell_length_b                   15.5703(8)
_cell_length_c                   18.9206(8)
_cell_measurement_temperature    95(2)
_cell_measurement_wavelength     0.49595
_cell_volume                     3822.4(3)
_computing_data_collection       'SAINT, Bruker AXS, 2003'
_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      95(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      '0.5 degree frames measured for 1 second each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49595
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42864
_diffrn_reflns_theta_full        20.32
_diffrn_reflns_theta_max         20.32
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    0.08
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, version 2.10 (Sheldrick)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         10864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.8539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                8923
_reflns_number_total             10864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818375a.txt
_cod_data_source_block           ChisholmCMC0525
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7104290