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_4325980
_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            'C30 H56 B4 Ca2 N12 O12'
_chemical_formula_weight         900.27
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                73.8910(10)
_cell_angle_beta                 80.4230(10)
_cell_angle_gamma                85.9690(10)
_cell_formula_units_Z            4
_cell_length_a                   14.7469(6)
_cell_length_b                   16.0986(6)
_cell_length_c                   21.3320(8)
_cell_measurement_reflns_used    8153
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.9
_cell_measurement_theta_min      2.3
_cell_volume                     4796.1(3)
_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 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0741
_diffrn_reflns_av_sigmaI/netI    0.1222
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            75459
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.301
_exptl_absorpt_correction_T_max  0.9534
_exptl_absorpt_correction_T_min  0.9151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.826
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         22400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1688
_refine_ls_R_factor_gt           0.0812
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1182P)^2^+2.5798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2200
_refine_ls_wR_factor_ref         0.2547
_reflns_number_gt                11555
_reflns_number_total             22400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012815_si_002_3.cif
_cod_data_source_block           xaly
_cod_database_code               4325980