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_4317389
_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            'C44 H56 I N12 Na'
_chemical_formula_weight         902.90
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.7483(8)
_cell_length_b                   10.7483(8)
_cell_length_c                   35.395(4)
_cell_measurement_reflns_used    5614
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.286
_cell_measurement_theta_min      2.262
_cell_volume                     3541.2(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            7795
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_correction_T_min  0.4708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0020(3)
_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   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0491P)^2^+0.0481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                1597
_reflns_number_total             1629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010690n_4.cif
_cod_data_source_block           {[HC(3,5-Me2pz)3]2Na}(I)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4317389