A homochiral 3D framework of mechanically interlocked 1D loops with solvent-dependent spin-state switching behaviors.
Sun, Xiao-Peng; Tang, Zheng; Yao, Zi-Shuo; Tao, Jun; Chemical communications (Cambridge, England) 56 (2020) 133–136; doi:10.1039/c9cc09063k

data_7125452
_publ_section_title
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 A homochiral 3D framework of mechanically interlocked 1D loops with
 solvent-dependent spin-state switching behaviors.
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_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              133
_journal_page_last               136
_journal_paper_doi               10.1039/c9cc09063k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C156 H124 B4 Fe2 N12 O16'
_chemical_formula_sum            'C156 H124 B4 Fe2 N12 O16'
_chemical_formula_weight         2577.60
_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             2019-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-15 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.028(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.080(6)
_cell_length_b                   16.715(6)
_cell_length_c                   32.015(8)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      50.154
_cell_measurement_theta_min      2.873
_cell_volume                     9299(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      160.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            46669
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        50.516
_diffrn_reflns_theta_max         50.516
_diffrn_reflns_theta_min         2.543
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0859 after correction.
The Ratio of minimum to maximum transmission is 0.8917.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.921
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 4171 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.056(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1695
_refine_ls_number_reflns         18288
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0834P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1619
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.871
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                13167
_reflns_number_total             18288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09063k2.cif
_cod_data_source_block           1CH3OH_160K
_cod_depositor_comments
'Adding full bibliography for 7125447--7125452.cif.'
_cod_database_code               7125452
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.766
_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 B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C155-C156
 2.22 with sigma of 0.01
 C155-O15
 1.55 with sigma of 0.01
 C156-O16
 1.41 with sigma of 0.01
 C155-O16
 1.35 with sigma of 0.01
 C1-N1
 1.11 with sigma of 0.01
3. Rigid bond restraints
 C1, B1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim B1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C155) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B4) = Uanis(B2)
Uanis(B1) = Uanis(B3)
5.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C73(H73A,H73B), C75(H75A,H75B), C77(H77A,H77B), C149(H14A,
 H14B), C151(H15D,H15E), C153(H15I,H15J), C155(H15N,H15O)
5.b Me refined with riding coordinates:
 C156(H15P,H15Q,H15R)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C13(H13), C14(H14), C18(H18),
 C19(H19), C22(H22), C23(H23), C25(H25), C27(H27), C28(H28), C33(H33), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C45(H45),
 C47(H47), C48(H48), C52(H52), C53(H53), C56(H56), C57(H57), C59(H59), C61(H61),
  C62(H62), C67(H67), C68(H68), C69(H69), C70(H70), C79(H79), C80(H80),
 C82(H82), C83(H83), C87(H87), C89(H89), C90(H90), C94(H94), C95(H95), C98(H98),
  C99(H99), C101(H101), C103(H103), C104(H104), C109(H109), C110(H110),
 C111(H111), C112(H112), C113(H113), C114(H114), C116(H116), C117(H117),
 C121(H121), C123(H123), C124(H124), C128(H128), C129(H129), C132(H132),
 C133(H133), C135(H135), C137(H137), C138(H138), C143(H143), C144(H144),
 C145(H145), C146(H146)
5.d Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C78(H78A,H78B,
 H78C), C150(H15A,H15B,H15C), C152(H15F,H15G,H15H), C154(H15K,H15L,H15M),
 B3(H3A,H3B,H3C), B4(H4A,H4B,H4C), B2(H2A,H2B,H2C), B1(H1A,H1B,H1C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 868.3 electrons were found in a volume of 3243.4\%A^3 in 1-CH^3^OH-160K void. This is consistent with the presence of about 12[CH3OH ] per formula unit which account for 864.0 electrons.
;
_shelx_res_checksum              43325
_shelx_fab_checksum              35129
_olex2_submission_special_instructions 'No special instructions were received'