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_4325978
_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            'C17 H30 B2 Ca N6 O2'
_chemical_formula_weight         412.17
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 104.5230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4290(4)
_cell_length_b                   14.4707(6)
_cell_length_c                   16.7495(7)
_cell_measurement_reflns_used    8083
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.5
_cell_volume                     2212.35(16)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         30.15
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.9411
_exptl_absorpt_correction_T_min  0.9189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       irregular
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         6531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.7042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                5191
_reflns_number_total             6531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012815_si_002_1.cif
_cod_data_source_block           xark
_cod_database_code               4325978