A flexible iron(ii) complex in which zero-field splitting is resistant to structural variation
Zadrozny, Joseph M.; Greer, Samuel M.; Hill, Stephen; Freedman, Danna E.; Chem. Sci. 7 (2016) 416–; doi:10.1039/C5SC02477C

data_1540750
_publ_section_title
;
 A flexible iron(ii) complex in which zero-field splitting is resistant to
 structural variation
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              416
_journal_paper_doi               10.1039/C5SC02477C
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         '(C6 Fe S10), 2(C16 H36 N)'
_chemical_formula_sum            'C38 H72 Fe N2 S10'
_chemical_formula_weight         933.43
_chemical_melting_point          ?
_chemical_name_common            (Bu4N)2[Fe(C3S5)2]
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2839 for OlexSys, GUI svn.r4713)
;
_audit_update_record
;
2015-05-08 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.509(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5730(5)
_cell_length_b                   32.0602(17)
_cell_length_c                   17.6411(9)
_cell_measurement_reflns_used    9748
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.40
_cell_volume                     4795.3(5)
_computing_cell_refinement       'SAINT v. 8.27 (Bruker, 2012)'
_computing_data_collection       'Apex2 v2.1-4'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87156
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_min         1.270
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.70a39
_exptl_absorpt_correction_T_min  0.6407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1238 before and 0.1057 after correction.
The Ratio of minimum to maximum transmission is 0.9102.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'red plate'
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.299
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+2.7409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7925
_reflns_number_total             9433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02477c2.cif
_cod_data_source_block           jz3045_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'unknown' was changed to '?' - the
value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               1540750
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C23(H23A,H23B), C35(H35A,H35B), C11(H11A,
 H11B), C31(H31A,H31B), C36(H36A,H36B), C29(H29A,H29B), C15(H15A,H15B),
 C19(H19A,H19B), C16(H16A,H16B), C32(H32A,H32B), C7(H7A,H7B), C20(H20A,H20B),
 C12(H12A,H12B), C37(H37A,H37B), C17(H17A,H17B), C8(H8A,H8B), C9(H9A,H9B),
 C24(H24A,H24B), C33(H33A,H33B), C13(H13A,H13B), C21(H21A,H21B), C25(H25A,H25B)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C38(H38A,H38B,H38C), C18(H18A,H18B,H18C), C34(H34A,H34B,
 H34C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C14(H14A,H14B,H14C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              50532
_shelx_shelxl_version_number     2014/7