Exploring secondary-sphere interactions in Fe-N x H y complexes relevant to N2 fixation.
Creutz, Sidney E.; Peters, Jonas C.; Chemical science 8 (2017) 2321–2328; doi:10.1039/c6sc04805f

data_1544758
_publ_section_title
;
 Exploring secondary-sphere interactions in Fe-N x H y complexes relevant
 to N2 fixation.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              2321
_journal_page_last               2328
_journal_paper_doi               10.1039/c6sc04805f
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C39 H51 Cl Fe N3 P3 Si'
_chemical_formula_weight         774.09
_chemical_name_common            'Compound 1''
_chemical_name_systematic        '[SiP(NMe)3]FeCl'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-10-24 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.962(2)
_cell_length_b                   11.0406(6)
_cell_length_c                   18.1487(9)
_cell_measurement_reflns_used    9069
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.55
_cell_measurement_theta_min      2.22
_cell_volume                     7806.9(7)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            150704
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.006
_diffrn_reflns_theta_min         1.533
_exptl_absorpt_coefficient_mu    0.640
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene, pentane'
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.147(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         24608
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0380P)^2^+8.6075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                22760
_reflns_number_total             24608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04805f2.cif
_cod_data_source_block           a14104_final
_cod_depositor_comments
;
 Adding full bibliography for 1544751--1544760.cif.

2019-02-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C78 H94 Cl2 Fe2 N6 P6 Si2'
_cod_original_formula_weight         1540.19
_cod_original_formula_units_Z            4
_cod_original_cell_volume        7807.0(7)
_cod_database_code               1544758
_shelxl_version_number           2013-3
_shelx_res_checksum              56879