A Five-Coordinate Phosphino/Acetate Iron(II) Scaffold That Binds N2, N2H2, N2H4, and NH3 in the Sixth Site
Caroline T. Saouma; Curtis E. Moore; Arnold L. Rheingold; Jonas C. Peters; Inorganic Chemistry 50 (2011) 11285–11287; doi:10.1021/ic2016066

data_4326895
_publ_section_title
;
 A Five-Coordinate Phosphino/Acetate Iron(II) Scaffold That Binds N2,
 N2H2, N2H4, and NH3 in the Sixth Site
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11285
_journal_page_last               11287
_journal_paper_doi               10.1021/ic2016066
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C68 H110 B Fe N O2 P3'
_chemical_formula_weight         1133.14
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.1960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5464(9)
_cell_length_b                   27.6742(18)
_cell_length_c                   17.3460(11)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.43
_cell_volume                     6465.4(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0988
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            121842
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.9658
_exptl_absorpt_correction_T_min  0.9175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             2468
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         18141
_refine_ls_number_restraints     633
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.7442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                12135
_reflns_number_total             18141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2016066_si_002_3.cif
_cod_data_source_block           Fe(NH3)
_cod_database_code               4326895