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_7000251
_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 I1 N6 O3 Zn1'
_chemical_formula_sum            'C24 H40 B I N6 O3 Zn'
_chemical_formula_weight         663.7
_chemical_name_common            'Chisholm 1604'
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
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_cell_length_b                   12.08910(10)
_cell_length_c                   34.8231(5)
_cell_measurement_reflns_used    2263
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     4407.44(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-97 (Sheldrick, 1997)'
_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      0.37708E-1
_diffrn_orient_matrix_UB_12      0.46557E-2
_diffrn_orient_matrix_UB_13      -0.259195E-1
_diffrn_orient_matrix_UB_21      0.870792E-1
_diffrn_orient_matrix_UB_22      0.395086E-1
_diffrn_orient_matrix_UB_23      0.117169E-1
_diffrn_orient_matrix_UB_31      -0.108906E-1
_diffrn_orient_matrix_UB_32      -0.86837E-1
_diffrn_orient_matrix_UB_33      0.39412E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            19579
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.921
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.5
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0259P)^2^+26.5815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                1858
_reflns_number_total             2265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812228h.txt
_cod_data_source_block           Chisholm1604
_cod_original_cell_volume        4407.43(8)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7000251