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_4317390
_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            'C32 H44 F6 K N12 P'
_chemical_formula_weight         780.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.291(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.144(4)
_cell_length_b                   13.377(6)
_cell_length_c                   15.988(7)
_cell_measurement_reflns_used    1496
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.244
_cell_measurement_theta_min      2.550
_cell_volume                     1954.1(15)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.1112
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8818
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0497
_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
  [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/
    [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0414P)^2^+0.0000sin\q/\l]
  where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                1471
_reflns_number_total             3463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010690n_5.cif
_cod_data_source_block           {[HC(3,5-Me2pz)3]2K}(PF6)
_cod_original_cell_volume        1954.2(14)
_cod_database_code               4317390