Syntheses and Solid State Structures of Tris(pyrazolyl)methane Complexes of Sodium, Potassium, Calcium, and Strontium: Comparison of Structures with Analogous Complexes of Lead(II)
Daniel L. Reger; Christine A. Little; Mark D. Smith; Arnold L. Rheingold; Louise M. Liable-Sands; Glen P. A. Yap; Ilia A. Guzei; Inorganic Chemistry 41 (2002) 19–27; doi:10.1021/ic010690n

data_4317391
_publ_section_title
;
 Syntheses and Solid State Structures of Tris(pyrazolyl)methane Complexes
 of Sodium, Potassium, Calcium, and Strontium: Comparison of Structures
 with Analogous Complexes of Lead(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              19
_journal_page_last               27
_journal_paper_doi               10.1021/ic010690n
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C90 H56 B2 F48 N12 O2 Sr'
_chemical_formula_weight         2358.71
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 90.3850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2709(7)
_cell_length_b                   13.2646(7)
_cell_length_c                   27.4189(13)
_cell_measurement_reflns_used    5886
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.088
_cell_measurement_theta_min      2.220
_cell_volume                     5190.2(4)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.611 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_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_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26615
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.8909
_exptl_absorpt_correction_T_min  0.7608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0017(6)
_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   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         9144
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0762
_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
  [0.00000+1.00000exp(0.50(sin\q/\l)^2^)]/
    [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.1657P)^2^+0.0000sin\q/\l]
  where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2159
_refine_ls_wR_factor_ref         0.2582
_reflns_number_gt                5039
_reflns_number_total             9144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010690n_6.cif
_cod_data_source_block           {[HC(pz)3]2((CH3)2CO)2Sr}{B[3,5-(CF3)2C6H3]4}2
_cod_database_code               4317391