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_4328022
_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(C19 H15 B N), 2(C2 H3 N)'
_chemical_formula_sum            'C68 H68 B2 Fe N16'
_chemical_formula_weight         1186.85
_chemical_name_systematic
; 
 bis(tris(5-methylpyrazolylmethane))iron(II) triphenylcyanoborate,
 acetonitrile solvate 
;
_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                 109.313(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.7202(10)
_cell_length_b                   10.2357(7)
_cell_length_c                   22.3913(15)
_cell_measurement_reflns_used    4019
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.47
_cell_volume                     3183.9(4)
_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 (Altomare et al., 1999)'
_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 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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41410
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            pink-red
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0540P)^2^+0.3287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                5132
_reflns_number_total             7307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2022038_si_002_1.cif
_cod_data_source_block           r1
_cod_database_code               4328022