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_4325979
_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            'C26 H44 B4 Ca2 N12 O2'
_chemical_formula_weight         680.13
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.260(2)
_cell_angle_beta                 102.222(2)
_cell_angle_gamma                105.636(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1854(6)
_cell_length_b                   12.8190(6)
_cell_length_c                   13.8733(7)
_cell_measurement_reflns_used    4096
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      21.5
_cell_measurement_theta_min      2.5
_cell_volume                     1862.33(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      250(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.969
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21912
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.9465
_exptl_absorpt_correction_T_min  0.9182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       'flat rhomboid'
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         8988
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+0.3175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2048
_reflns_number_gt                4890
_reflns_number_total             8988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012815_si_002_2.cif
_cod_data_source_block           xkar
_cod_database_code               4325979