Spin-crossover iron(ii) long-chain complex with slow spin equilibrium at low temperatures.
Zhao, Qi; Xue, Jin-Peng; Liu, Zhi-Kun; Yao, Zi-Shuo; Tao, Jun; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11106–11112; doi:10.1039/d1dt01378e

data_7707799
_publ_section_title
;
 Spin-crossover iron(ii) long-chain complex with slow spin equilibrium at
 low temperatures.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11106
_journal_page_last               11112
_journal_paper_doi               10.1039/d1dt01378e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H60 B2 Fe N10'
_chemical_formula_sum            'C40 H60 B2 Fe N10'
_chemical_formula_weight         758.45
_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   mixed
_audit_creation_date             2021-06-03
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.05.19 svn.r3ea446d0 for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-07-01 deposited with the CCDC.	2021-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.678(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.5280(10)
_cell_length_b                   22.6959(19)
_cell_length_c                   35.720(3)
_cell_measurement_reflns_used    4251
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8960
_cell_measurement_theta_min      3.8300
_cell_volume                     8525.7(13)
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1746
_diffrn_reflns_av_unetI/netI     0.1280
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            66606
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         3.531
_exptl_absorpt_coefficient_mu    0.394
_exptl_crystal_colour            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       plate
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1065
_refine_ls_number_reflns         15342
_refine_ls_number_restraints     370
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0789P)^2^+6.6486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9118
_reflns_number_total             15342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01378e2.cif
_cod_data_source_block           complex1
_cod_depositor_comments          'Adding full bibliography for 7707799.cif.'
_cod_original_cell_volume        8525.6(12)
_cod_database_code               7707799
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C58A, C58B}
3. Restrained distances
 C58A-C59A = C60A-C59A = C61A-C60A = C62A-C61A = C62A-C63A = C64A-C63A = C65A-
 C64A = C65A-C66A
 1.52 with sigma of 0.02
 C59B-C58B = C60B-C59B = C60B-C61B = C62B-C61B = C63B-C62B = C63B-C64B = C64B-
 C65B = C66B-C65B
 1.52 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C55 \\sim C58B \\sim C60B \\sim C66B \\sim C63B \\sim C59B \\sim C65B \\sim
C62B \\sim C64B \\sim C61B \\sim C59A \\sim C60A \\sim C65A \\sim C63A \\sim
C64A \\sim C61A \\sim C66A \\sim C58A \\sim C62A: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.02 within 2A
Uanis(C58A) = Uanis(C58B)
5. Rigid body (RIGU) restrains
 C55, C58B, C60B, C66B, C63B, C59B, C65B, C62B, C64B, C61B, C59A, C60A, C65A,
 C63A, C64A, C61A, C66A, C58A, C62A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Others
 Sof(C58B)=Sof(H58A)=Sof(H58B)=Sof(C60B)=Sof(H60C)=Sof(H60D)=Sof(C59B)=
 Sof(H59C)=Sof(H59D)=Sof(C62B)=Sof(H62C)=Sof(H62D)=Sof(C61B)=Sof(H61C)=
 Sof(H61D)=Sof(C65B)=Sof(H65C)=Sof(H65D)=Sof(C66B)=Sof(H66D)=Sof(H66E)=
 Sof(H66F)=Sof(C63B)=Sof(H63C)=Sof(H63D)=Sof(C64B)=Sof(H64C)=Sof(H64D)=1-FVAR(1)
 Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(C63A)=
 Sof(H63A)=Sof(H63B)=Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(C62A)=Sof(H62A)=
 Sof(H62B)=Sof(C64A)=Sof(H64A)=Sof(H64B)=Sof(C65A)=Sof(H65A)=Sof(H65B)=
 Sof(C66A)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C58A)=Sof(H58C)=Sof(H58D)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C72(H72A,H72B), C32(H32A,H32B), C75(H75A,H75B), C58B(H58A,
 H58B), C21(H21A,H21B), C73(H73A,H73B), C34(H34A,H34B), C20(H20A,H20B),
 C35(H35A,H35B), C74(H74A,H74B), C76(H76A,H76B), C19(H19A,H19B), C33(H33A,H33B),
  C36(H36A,H36B), C22(H22A,H22B), C77(H77A,H77B), C78(H78A,H78B), C38(H38A,
 H38B), C37(H37A,H37B), C23(H23A,H23B), C39(H39A,H39B), C24(H24A,H24B),
 C79(H79A,H79B), C25(H25A,H25B), C59A(H59A,H59B), C60A(H60A,H60B), C63A(H63A,
 H63B), C61A(H61A,H61B), C62A(H62A,H62B), C64A(H64A,H64B), C65A(H65A,H65B),
 C60B(H60C,H60D), C59B(H59C,H59D), C62B(H62C,H62D), C61B(H61C,H61D), C65B(H65C,
 H65D), C63B(H63C,H63D), C64B(H64C,H64D), C58A(H58C,H58D)
7.b Aromatic/amide H refined with riding coordinates:
 C68(H68), C13(H13), C28(H28), C14(H14), C47(H47), C7(H7), C70(H70), C54(H54),
 C31(H31), C30(H30), C71(H71), C56(H56), C16(H16), C48(H48), C49(H49), C46(H46),
  C8(H8), C43(H43), C9(H9), C52(H52), C44(H44), C51(H51), C41(H41), C6(H6),
 C12(H12), C5(H5), C10(H10), C42(H42), C50(H50), C45(H45), C1(H1), C4(H4),
 C11(H11), C3(H3), C2(H2), C53(H53)
7.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C80(H80A,H80B,H80C), C26(H26A,H26B,H26C), C66A(H66A,H66B,
 H66C), C66B(H66D,H66E,H66F)
;
_shelx_res_checksum              41646
_olex2_submission_special_instructions 'No special instructions were received'