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_1544759
_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            'C33 H45 Cl0 Fe N5 P3 Si'
_chemical_formula_weight         688.59
_chemical_name_common            'Compound 2''
_chemical_name_systematic        '[SiP(NMe)3]FeN2'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 91.270(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6457(5)
_cell_length_b                   19.2443(9)
_cell_length_c                   16.2208(8)
_cell_measurement_reflns_used    9681
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.19
_cell_volume                     3322.3(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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  0.0531
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            126704
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.343
_diffrn_reflns_theta_min         1.256
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_refine_diff_density_max         1.658
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.027(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         16433
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0587P)^2^+3.1175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                15438
_reflns_number_total             16433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04805f2.cif
_cod_data_source_block           a14107_final
_cod_depositor_comments
;Adding full bibliography for 1544751--1544760.cif.

 Adding full bibliography for 1544751--1544760.cif.
;
_cod_database_code               1544759
_shelxl_version_number           2013-3
_shelx_res_checksum              58445