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_1540748
_publ_section_title
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 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_absolute_configuration ad
_chemical_formula_moiety         'C22 H32 Fe K O7 S10, C20 H40 K O8'
_chemical_formula_sum            'C42 H72 Fe K2 O15 S10'
_chemical_formula_weight         1271.65
_chemical_name_common            '[(18-crown-6)K]2[Fe(C3S5)2]'
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-08 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.302(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6660(4)
_cell_length_b                   17.7362(8)
_cell_length_c                   17.9259(7)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100.08
_cell_volume                     2977.9(2)
_computing_cell_refinement       'SAINT v.7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.08
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            52038
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.422
_diffrn_reflns_theta_min         1.148
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0533 before and 0.0477 after correction.
The Ratio of minimum to maximum transmission is 0.9564.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details
;
 Flack x determined using 4180 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_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     623
_refine_ls_number_reflns         11046
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0811P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.816
_reflns_Friedel_fraction_max     0.808
_reflns_number_gt                10121
_reflns_number_total             11046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02477c2.cif
_cod_data_source_block           jz3078_0m
_cod_database_code               1540748
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C39-C41 \\sim C47-C49 \\sim C40-C42 \\sim C50-C48
 with sigma of 0.02
 C45-C43 \\sim C44-C46 \\sim C38-C36 \\sim C37-C35
 with sigma of 0.02
 C45-C44 \\sim C37-C36
 with sigma of 0.02
 C48-C49 \\sim C40-C41
 with sigma of 0.02
 C47-C49 \\sim C48-C50 \\sim C39-C41 \\sim C40-C42
 with sigma of 0.02
 C38-O15 \\sim O15-C35
 with sigma of 0.02
 C46-O14 \\sim O14-C43
 with sigma of 0.02
 C35-O15 \\sim C46-O14
 with sigma of 0.02
 C50-O17 \\sim O17-C47
 with sigma of 0.02
 C39-O16 \\sim O16-C42
 with sigma of 0.02
 C47-C50 \\sim C42-C39
 with sigma of 0.02
 C38-C35 \\sim C43-C46
 with sigma of 0.02
3. Others
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(O14)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C43)=
 Sof(H43A)=Sof(H43B)=Sof(C45)=Sof(H45A)=Sof(H45B)=1-FVAR(1)
 Sof(O15)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=
 Sof(H38A)=Sof(H38B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(1)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C48)=Sof(H48A)=
 Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(O17)=1-FVAR(2)
 Sof(O16)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C18(H18A,H18B), C29(H29A,H29B), C16(H16A,H16B), C13(H13A,H13B),
 C25(H25A,H25B), C9(H9A,H9B), C7(H7A,H7B), C22(H22A,H22B), C30(H30A,H30B),
 C21(H21A,H21B), C14(H14A,H14B), C17(H17A,H17B), C27(H27A,H27B), C26(H26A,H26B),
  C11(H11A,H11B), C24(H24A,H24B), C28(H28A,H28B), C12(H12A,H12B), C15(H15A,
 H15B), C10(H10A,H10B), C20(H20A,H20B), C32(H32A,H32B), C23(H23A,H23B),
 C33(H33A,H33B), C31(H31A,H31B), C19(H19A,H19B), C34(H34A,H34B), C40(H40A,H40B),
  C35(H35A,H35B), C37(H37A,H37B), C41(H41A,H41B), C38(H38A,H38B), C42(H42A,
 H42B), C36(H36A,H36B), C39(H39A,H39B), C46(H46A,H46B), C44(H44A,H44B),
 C43(H43A,H43B), C45(H45A,H45B), C47(H47A,H47B), C50(H50A,H50B), C48(H48A,H48B),
  C49(H49A,H49B)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'