Catalytic Nitrogen-to-Ammonia Conversion by Osmium and Ruthenium Complexes.
Fajardo, Jr, Javier; Peters, Jonas C.; Journal of the American Chemical Society 139 (2017) 16105–16108; doi:10.1021/jacs.7b10204

data_4131757
_publ_section_title
;
 Catalytic Nitrogen-to-Ammonia Conversion by Osmium and Ruthenium
 Complexes.
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16105
_journal_page_last               16108
_journal_paper_doi               10.1021/jacs.7b10204
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C36 H56 N2 Os P3 Si, C F3 O3 S'
_chemical_formula_sum            'C37 H56 F3 N2 O3 Os P3 S Si'
_chemical_formula_weight         977.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2348(15)
_cell_length_b                   12.2611(7)
_cell_length_c                   15.1377(9)
_cell_measurement_reflns_used    9390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.73
_cell_measurement_theta_min      2.81
_cell_volume                     4126.9(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59454
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.020
_diffrn_reflns_theta_min         2.326
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.337
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0879 before and 0.0770 after correction. The Ratio of minimum to maximum transmission is 0.8810. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         13119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0291
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0497
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                11805
_reflns_number_total             13119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10204_si_002.cif
_cod_data_source_block           jfj_final_orthorhombic
_cod_database_code               4131757
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.628
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.991(4)
 0.009(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C8AA(H8AA), C10(H10), C15(H15), C1BA(H1BA), C11(H11), C17(H17)
3.b Aromatic/amide H refined with riding coordinates:
 C6AA(H6AA), C0AA(H0AA), C3BA(H3BA), C4AA(H4AA), C1AA(H1AA), C13(H13),
 C2AA(H2AA), C16(H16), C12(H12), C14(H14), C9AA(H9AA), C9BA(H9BA)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C7BA(H7BA,H7BB,H7BC), C7AA(H7AA,H7AB,H7AC), C2BA(H2BA,H2BB,
 H2BC), C0BA(H0BA,H0BB,H0BC), C4BA(H4BA,H4BB,H4BC), C5BA(H5BA,H5BB,H5BC),
 C6BA(H6BA,H6BB,H6BC), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C19(H19C,H19D,
 H19E), C8BA(H8BA,H8BB,H8BC)
;
_shelx_res_checksum              89370
_shelx_hkl_checksum              88428
_olex2_submission_special_instructions 'No special instructions were received'