H<sub>2</sub> Binding, Splitting, and Net Hydrogen Atom Transfer at a Paramagnetic Iron Complex.
Prokopchuk, Demyan E.; Chambers, Geoffrey M.; Walter, Eric D.; Mock, Michael T.; Bullock, R. Morris; Journal of the American Chemical Society 141 (2019) 1871–1876; doi:10.1021/jacs.8b12823

data_4127915
_publ_section_title
;
 H<sub>2</sub> Binding, Splitting, and Net Hydrogen Atom Transfer at a
 Paramagnetic Iron Complex.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1871
_journal_page_last               1876
_journal_paper_doi               10.1021/jacs.8b12823
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C44 H48 Fe N2 P4'
_chemical_formula_sum            'C56 H74 Fe N2 O P4'
_chemical_formula_weight         970.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.50(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.86(4)
_cell_length_b                   11.175(11)
_cell_length_c                   23.40(2)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.990
_cell_measurement_theta_min      2.235
_cell_volume                     8538(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            119924
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.213
_diffrn_reflns_theta_min         1.840
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.9931
_exptl_absorpt_correction_T_min  0.7749
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0657 before and 0.0464 after correction. The Ratio of minimum to maximum transmission is 0.7803. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.759
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         11528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+8.0901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9929
_reflns_number_total             11528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12823_si_002.cif
_cod_data_source_block           15_73
_cod_original_cell_volume        8539(15)
_cod_database_code               4127915
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H26A,H26B} of C26, {H25A,H25B} of C25, {H28A,H28B} of C28,
   {H29A,H29B} of C29, {H27A,H27B} of C27, {H30A,H30B} of C30, {H32A,H32B} of
  C32, {H31A,H31B} of C31
 At 1.5 times of:
  {H,HA} of C22
2.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C27(H27A,
 H27B), C30(H30A,H30B), C32(H32A,H32B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C14(H14), C17(H17), C15(H15), C16(H16), C6(H6), C5(H5), C4(H4),
 C40(H40), C42(H42), C2(H2), C20(H20), C37(H37), C38(H38), C24(H24), C34(H34),
 C3(H3), C44(H44), C12(H12), C43(H43), C8(H8), C23(H23), C41(H41), C36(H36),
 C11(H11), C35(H35), C9(H9), C21(H21), C10(H10), C22(H22)
;
_shelx_res_checksum              33551
_shelx_hkl_checksum              35026
_shelx_fab_checksum              93230
_olex2_submission_special_instructions 'No special instructions were received'