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_4131758
_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 H54 Os P3 Si'
_chemical_formula_sum            'C36 H54 Os P3 Si'
_chemical_formula_weight         797.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                100.081(6)
_cell_angle_beta                 94.097(6)
_cell_angle_gamma                118.576(5)
_cell_formula_units_Z            2
_cell_length_a                   11.1667(18)
_cell_length_b                   11.2875(18)
_cell_length_c                   16.677(3)
_cell_measurement_reflns_used    9586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.67
_cell_measurement_theta_min      3.19
_cell_volume                     1788.0(5)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.06
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 1.000
_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  0.0727
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            426246
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         47.759
_diffrn_reflns_theta_min         2.396
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.757
_exptl_absorpt_correction_T_max  0.7503
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1008 before and 0.0918 after correction. The Ratio of minimum to maximum transmission is 0.8721. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.145
_refine_diff_density_max         3.090
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         33848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.2530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31137
_reflns_number_total             33848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10204_si_003.cif
_cod_data_source_block           nix_jfj_39runs
_cod_database_code               4131758
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.612
_shelx_estimated_absorpt_t_min   0.519
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C006(H006), C00A(H00G), C00C(H00H), C00P(H00), C00Q(H0AA), C00U(H4AA)
2.b Aromatic/amide H refined with riding coordinates:
 C00G(H00I), C00M(H00V), C00O(H00Z), C00R(H1AA), C00S(H2AA), C00T(H3AA),
 C00V(H5AA), C00X(H7AA), C00Y(H8AA), C00Z(H9AA), C010(H010), C011(H011)
2.c Idealised Me refined as rotating group:
 C007(H00A,H00B,H00C), C009(H00D,H00E,H00F), C00H(H00J,H00K,H00L), C00I(H00M,
 H00N,H00O), C00K(H00P,H00Q,H00R), C00L(H00S,H00T,H00U), C00N(H00W,H00X,H00Y),
 C00W(H6AA,H,HA), C012(H01A,H01B,H01C), C013(H01D,H01E,H01F), C014(H01G,H01H,
 H01I), C015(H01J,H01K,H01L)
;
_shelx_res_checksum              45290
_shelx_hkl_checksum              15706
_olex2_submission_special_instructions 'No special instructions were received'