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_7237022
_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_formula_moiety         'C18 H16 Br2 Fe N10'
_chemical_formula_sum            'C18 H16 Br2 Fe N10'
_chemical_formula_weight         588.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-10-30 deposited with the CCDC.
2018-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.212(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7407(9)
_cell_length_b                   12.4108(13)
_cell_length_c                   19.0055(19)
_cell_measurement_reflns_used    4935
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.1766
_cell_measurement_theta_min      2.9902
_cell_volume                     2056.1(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15769
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.164
_diffrn_reflns_theta_max         25.164
_diffrn_reflns_theta_min         2.856
_exptl_absorpt_coefficient_mu    4.650
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS Inc., Madison, Wisconsin, USA'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.900
_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         0.574
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0403
_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^)+8.7119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2589
_reflns_number_total             3581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7tc05111e2.cif
_cod_data_source_block           beta-123K
_cod_database_code               7237022
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N3(H3), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C6(H6A,H6B), C9(H9A,H9B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C11(H11), C1(H1), C3(H3A), C12(H12), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'