Synthesis and Characterization of Di- and Trivalent Pyrazolylborate β-Diketonates and Cyanometalates
Minao Tang; Dongfeng Li; Uma Prasad Mallik; Yuan-Zhu Zhang; Rodolphe Clérac; Gordon T. Yee; Myung-Hwan Whangbo; Amshumali Mungalimane; Stephen M. Holmes; Inorganic Chemistry 50 (2011) 5153–5164; doi:10.1021/ic200464t

data_4325267
_publ_section_title
;
 Synthesis and Characterization of Di- and Trivalent Pyrazolylborate
 \b-Diketonates and Cyanometalates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5153
_journal_page_last               5164
_journal_paper_doi               10.1021/ic200464t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C29 H49 B Mn N8 O2'
_chemical_formula_weight         607.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.026(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4389(5)
_cell_length_b                   22.3831(10)
_cell_length_c                   12.9427(6)
_cell_measurement_reflns_used    8485
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      67.96
_cell_measurement_theta_min      3.95
_cell_volume                     3311.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22040
_diffrn_reflns_theta_full        59.00
_diffrn_reflns_theta_max         59.00
_diffrn_reflns_theta_min         3.95
_exptl_absorpt_coefficient_mu    3.536
_exptl_absorpt_correction_T_max  0.7774
_exptl_absorpt_correction_T_min  0.6191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs in APEX 2 (Brukerxs,2005)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.0011(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0758
_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^)+(0.1821P)^2^+18.3112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2374
_refine_ls_wR_factor_ref         0.2964
_reflns_number_gt                3865
_reflns_number_total             4461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200464t_si_002_1.cif
_cod_data_source_block           1_x05085
_cod_database_code               4325267