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_4325272
_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            'C54 H52 B Mn N10 P2'
_chemical_formula_weight         968.75
_chemical_name_common            '[PPN][(Tp*)Mn(CN)3]'
_chemical_name_systematic
; 
 ? 
;
_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                84.4993(8)
_cell_angle_beta                 85.7660(8)
_cell_angle_gamma                82.9083(9)
_cell_formula_units_Z            2
_cell_length_a                   9.7995(2)
_cell_length_b                   15.7266(3)
_cell_length_c                   16.3355(4)
_cell_measurement_reflns_used    35846
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2481.84(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0799
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51753
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'scalepack (otwinowski & Minor, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         11390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0859P)^2^+1.0266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1728
_reflns_number_gt                7474
_reflns_number_total             11390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200464t_si_002_6.cif
_cod_data_source_block           8_k07314
_cod_database_code               4325272