Synthesis and coordination chemistry of TpC*MI complexes where M = Mg, Ca, Sr, Ba and Zn and TpC* = tris[3-(2-methoxy-1,1-dimethyl)pyrazolyl]hydroborate
Chisholm, Malcolm H.; Gallucci, Judith C.; Yaman, Gulsah; Dalton Transactions  (2009) 368–374; doi:10.1039/b812228h

data_7000247
_publ_section_title
;
 Synthesis and coordination chemistry of TpC*MI complexes where M = Mg,
 Ca, Sr, Ba and Zn and TpC* =
 tris[3-(2-methoxy-1,1-dimethyl)pyrazolyl]hydroborate
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              368
_journal_page_last               374
_journal_paper_doi               10.1039/b812228h
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H40 B1 Mg1 N6 O3, C6 H6, I'
_chemical_formula_sum            'C30 H46 B I Mg N6 O3'
_chemical_formula_weight         700.75
_chemical_name_common            'Chisholm 1609'
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      198
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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             2008-05-28T14:49:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9023(2)
_cell_length_b                   14.9023(2)
_cell_length_c                   14.9023(2)
_cell_measurement_reflns_used    1109
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     3309.48(8)
_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-7 (Sheldrick, 197)'
_diffrn_ambient_temperature      150(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       'phi and omega scans''
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.520958E-1
_diffrn_orient_matrix_UB_12      -0.263055E-1
_diffrn_orient_matrix_UB_13      0.331204E-1
_diffrn_orient_matrix_UB_21      0.191835E-1
_diffrn_orient_matrix_UB_22      -0.615264E-1
_diffrn_orient_matrix_UB_23      -0.186925E-1
_diffrn_orient_matrix_UB_31      0.376953E-1
_diffrn_orient_matrix_UB_32      -0.50435E-2
_diffrn_orient_matrix_UB_33      0.55286E-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  0.049
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28583
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.37
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular chunk'
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.33
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1965
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+4.0481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                1907
_reflns_number_total             1965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812228h.txt
_cod_data_source_block           Chisholm1609
_cod_original_sg_symbol_H-M      P213
_cod_database_code               7000247