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_7000250
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H40 B1 Ba1 I1 N6 O3, C3.5 H4'
_chemical_formula_sum            'C27.5 H44 B Ba I N6 O3'
_chemical_formula_weight         781.74
_chemical_name_common            'Chisholm 1539'
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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             2008-07-08T14:39:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.575(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.3403(2)
_cell_length_b                   12.3916(1)
_cell_length_c                   26.6151(2)
_cell_measurement_reflns_used    7860
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     6631.33(10)
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_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      0.132053E-1
_diffrn_orient_matrix_UB_12      -0.3961E-3
_diffrn_orient_matrix_UB_13      -0.479474E-1
_diffrn_orient_matrix_UB_21      0.61833E-1
_diffrn_orient_matrix_UB_22      -0.488388E-1
_diffrn_orient_matrix_UB_23      0.17433E-1
_diffrn_orient_matrix_UB_31      -0.184388E-1
_diffrn_orient_matrix_UB_32      -0.300158E-1
_diffrn_orient_matrix_UB_33      -0.18689E-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  0.052
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            55260
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.165
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.515
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         13433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+164.5556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                10175
_reflns_number_total             13433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812228h.txt
_cod_data_source_block           Chisholm1539
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C27.50 H44 B Ba I N6 O3'
_cod_database_code               7000250