Bimetallic iron-tin catalyst for N<sub>2</sub> to NH<sub>3</sub> and a silyldiazenido model intermediate.
Dorantes, Michael J.; Moore, James T.; Bill, Eckhard; Mienert, Bernd; Lu, Connie C.; Chemical communications (Cambridge, England) 56 (2020) 11030–11033; doi:10.1039/d0cc04563b

data_7127011
_publ_section_title
;
 Bimetallic iron-tin catalyst for N<sub>2</sub> to NH<sub>3</sub> and a
 silyldiazenido model intermediate.
;
_journal_issue                   75
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11030
_journal_page_last               11033
_journal_paper_doi               10.1039/d0cc04563b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C39 H60 N4 P3 Sn, C12 H24 Li O3, C4 H8 O'
_chemical_formula_sum            'C55 H92 Li N4 O4 P3 Sn'
_chemical_formula_weight         1091.86
_chemical_name_common            '17092; (THF)3LiSnL'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc25d9xt
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-06-03 deposited with the CCDC.	2020-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.6945(8)
_cell_length_b                   13.6945(8)
_cell_length_c                   18.3276(11)
_cell_measurement_reflns_used    2931
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.81
_cell_volume                     2976.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ShelXle Rev. 836 (Huebschle, 2011)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker PHOTON-II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78284
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.606
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'I\uS 3.0 Microfocus Tube'
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
; 
 Flack x determined using 1705 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.010(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5996
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+2.8695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                4622
_reflns_number_total             5996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04563b3.cif
_cod_data_source_block           (THF)3LiSnL_17092
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7127010--7127013.cif.
;
_cod_original_cell_volume        2976.7(4)
_cod_database_code               7127011
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              25764