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_7127012
_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         'C43 H68 Fe K N6 O P3 Sn'
_chemical_formula_sum            'C43 H68 Fe K N6 O P3 Sn'
_chemical_formula_weight         991.58
_chemical_name_common            '19031; 2, K[LSnFeN2]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc25d9vr
_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                90
_cell_formula_units_Z            4
_cell_length_a                   19.5107(9)
_cell_length_b                   10.8907(6)
_cell_length_c                   21.8866(10)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.35
_cell_measurement_theta_min      2.29
_cell_volume                     4650.6(4)
_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    'SHELXT-2014/5 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39072
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.560
_diffrn_reflns_theta_min         2.639
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6522
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
; 
 Flack x determined using 4634 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.019(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         14075
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+8.6870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                11642
_reflns_number_total             14075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04563b3.cif
_cod_data_source_block           2_KLSnFeN2_19148
_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_database_code               7127012
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              35338