Efficient Hydride and Pyrazolyl Redistribution upon Thermolysis of a Calcium Complex Containing Dihydrobis(pyrazolyl)borate Ligands
Mark J. Saly; Jing Li; Mary Jane Heeg; Charles H. Winter; Inorganic Chemistry 50 (2011) 7385–7387; doi:10.1021/ic2012815

data_4325981
_publ_section_title
;
 Efficient Hydride and Pyrazolyl Redistribution upon Thermolysis of a
 Calcium Complex Containing Dihydrobis(pyrazolyl)borate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7385
_journal_page_last               7387
_journal_paper_doi               10.1021/ic2012815
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C47 H81 B7 Ca3 N18 O13'
_chemical_formula_weight         1302.21
_chemical_name_systematic
; 
 ? 
;
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_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
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_cell_length_b                   16.9880(4)
_cell_length_c                   13.5711(4)
_cell_measurement_reflns_used    5312
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_cell_measurement_theta_min      2.4
_cell_volume                     3391.80(15)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       'Bruker APEX2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
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_diffrn_reflns_limit_h_max       0
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_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.9695
_exptl_absorpt_correction_T_min  0.9318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       rods
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.306
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2920
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.7758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                2074
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012815_si_002_4.cif
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