Multiple spin phases in a switchable Fe(ii) complex: polymorphism and symmetry breaking effects
Hang, Hao; Fei, Bin; Chen, Xiu Qin; Tong, Ming Liang; Ksenofontov, Vadim; Gural'skiy, Il’ya A.; Bao, Xin; Journal of Materials Chemistry C 6 (2018) 3352–; doi:10.1039/C7TC05111E

data_7237023
_publ_section_title
;
 Multiple spin phases in a switchable Fe(ii) complex: polymorphism and
 symmetry breaking effects
;
_journal_issue                   13
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              3352
_journal_paper_doi               10.1039/C7TC05111E
_journal_volume                  6
_journal_year                    2018
_chemical_absolute_configuration unknow
_chemical_formula_moiety         '2(C18 H16 Br2 Fe N10)'
_chemical_formula_sum            'C36 H32 Br4 Fe2 N20'
_chemical_formula_weight         1176.15
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-10-30 deposited with the CCDC.
2018-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.534(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8548(5)
_cell_length_b                   12.5141(7)
_cell_length_c                   19.2074(11)
_cell_measurement_reflns_used    5429
_cell_measurement_temperature    146(2)
_cell_measurement_theta_max      26.2127
_cell_measurement_theta_min      2.8217
_cell_volume                     2124.3(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      146.1
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_number            7464
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_min         2.822
_exptl_absorpt_coefficient_mu    4.501
_exptl_absorpt_correction_T_max  0.7878
_exptl_absorpt_correction_T_min  0.5411
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166'
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.190(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         7464
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0316P)^2^+0.7047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                5271
_reflns_number_total             7464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7tc05111e2.cif
_cod_data_source_block           beta-146K
_cod_database_code               7237023
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.810(19) 0.190(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Restrained distances
 N3-C8B = N2-C7B
 1.48 with sigma of 0.02
 C7B-C8B = C7A-C8A
 1.5 with sigma of 0.02
 N3-C8A = N2-C7A
 1.48 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C36) = Uanis(C34)
Uanis(C21) = Uanis(C19)
Uanis(C18) = Uanis(C16)
Uanis(C7B) = Uanis(C8A) = Uanis(C8B) = Uanis(C7A) = Uanis(C25) = Uanis(C26)
Uanis(C33) = Uanis(C35)
5. Others
 Fixed Sof: C8A(0.68979) H8AA(0.68979) H8AB(0.68979) C7A(0.68979)
 H7AA(0.68979) H7AB(0.68979) C8B(0.31021) H8BA(0.31021) H8BB(0.31021)
 C7B(0.31021) H7BA(0.31021) H7BB(0.31021)
6.a Ternary CH refined with riding coordinates:
 N2(H2), N12(H12A), N13(H13), N3(H3A)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C24(H24A,H24B),
 C6(H6A,H6B), C8A(H8AA,H8AB), C7A(H7AA,H7AB), C8B(H8BA,H8BB), C7B(H7BA,H7BB)
6.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C3(H3), C19(H19), C32(H32), C22(H22), C4(H4), C1(H1), C29(H29),
 C30(H30), C14(H14), C12(H12), C11(H11)
;
_shelx_res_checksum              51217
_shelx_hkl_checksum              12748
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'