Tris(5-methylpyrazolyl)methane: Synthesis and Properties of Its Iron(II) Complex
Margaret A. Goodman; Alexander Y. Nazarenko; Barbara J. Casavant; Zhanjie Li; William W. Brennessel; Michael J. DeMarco; Gen Long; M. Scott Goodman; Inorganic Chemistry 51 (2012) 1084–1093; doi:10.1021/ic2022038

data_4328030
_publ_section_title
;
 Tris(5-methylpyrazolyl)methane: Synthesis and Properties of Its Iron(II)
 Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1084
_journal_page_last               1093
_journal_paper_doi               10.1021/ic2022038
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C26 H32 Fe N12, 2(Cl O4)'
_chemical_formula_sum            'C26 H32 Cl2 Fe N12 O8'
_chemical_formula_weight         767.39
_chemical_name_systematic
;
  bis(tris(5-methylpyrazolylmethane))iron(II) perchlorate
;
_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                   11.2103(6)
_cell_length_b                   11.2103(6)
_cell_length_c                   21.708(2)
_cell_measurement_reflns_used    3817
_cell_measurement_temperature    300.0(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.30
_cell_volume                     2362.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Sheldrick, 1999)'
_diffrn_ambient_temperature      300.0(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10233
_diffrn_reflns_theta_full        32.55
_diffrn_reflns_theta_max         32.55
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0510
_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^)+(0.1057P)^2^+0.6544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                1382
_reflns_number_total             1901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2022038_si_002_9.cif
_cod_data_source_block           ra11
_cod_original_cell_volume        2362.5(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4328030