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_7237021
_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
_audit_creation_date             2017-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-08 deposited with the CCDC.
2018-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.267(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7376(19)
_cell_length_b                   12.499(2)
_cell_length_c                   19.217(4)
_cell_measurement_reflns_used    4434
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.3258
_cell_measurement_theta_min      2.9923
_cell_volume                     2095.3(7)
_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      298.6
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16896
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        24.782
_diffrn_reflns_theta_max         24.782
_diffrn_reflns_theta_min         2.992
_exptl_absorpt_coefficient_mu    4.563
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS Inc., Madison, Wisconsin, USA'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.864
_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         0.624
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3484
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0002P)^2^+16.7011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2219
_reflns_number_total             3484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7tc05111e2.cif
_cod_data_source_block           beta-RT
_cod_original_cell_volume        2095.4(7)
_cod_database_code               7237021
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details   'SADABS (Bruker, 2014)'
_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. Restrained distances
 C8A-C7A \\sim C8-C7
 with sigma of 0.02
 N3-C8 \\sim N3-C8A \\sim N2-C7A \\sim N2-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C8A)
Uanis(C7A) = Uanis(C7)
4. Others
 Fixed Sof: C7(0.68) H7A(0.68) H7B(0.68) C8(0.68) H8A(0.68) H8B(0.68)
 C8A(0.32) H8AA(0.32) H8AB(0.32) C7A(0.32) H7AA(0.32) H7AB(0.32)
5.a Ternary CH refined with riding coordinates:
 N3(H3), N2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C9(H9A,H9B), C7(H7A,H7B), C8(H8A,H8B), C8A(H8AA,H8AB), C7A(H7AA,
 H7AB)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C1(H1), C4(H4), C14(H14), C11(H11), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'