Crystal structures and the ferroelectric properties of homochiral metal-organic frameworks constructed from a single chiral ligand.
Xu, Xuebin; Liu, Meiying; Liu, Zhiliang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10402–10406; doi:10.1039/d0dt01323d

data_7704728
_publ_section_title
;
 Crystal structures and the ferroelectric properties of homochiral
 metal-organic frameworks constructed from a single chiral ligand.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10402
_journal_page_last               10406
_journal_paper_doi               10.1039/d0dt01323d
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H28 Co N4 O5'
_chemical_formula_sum            'C28 H28 Co N4 O5'
_chemical_formula_weight         559.47
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-24 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.936(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3218(7)
_cell_length_b                   24.686(3)
_cell_length_c                   9.3234(11)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.37
_cell_volume                     1428.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      273.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20232
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.400
_diffrn_reflns_theta_min         1.650
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0707 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.9418.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 3135 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         7133
_refine_ls_number_restraints     672
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0651P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                6805
_reflns_number_total             7133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01323d2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'AD' was changed
to 'ad' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7704728--7704729.cif.

 Adding full bibliography for 7704728--7704729.cif.
;
_cod_database_code               7704728
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.831
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2-C6 \\sim O2-C29
 with sigma of 0.02
 N3-C12 \\sim N5-C32
 with sigma of 0.02
 N3-C19 \\sim N5-C33
 with sigma of 0.02
 O5-C6 \\sim O6-C29
 with sigma of 0.02
 N4-C9 \\sim N6-C30
 with sigma of 0.02
 N4-C28 \\sim N6-C42
 with sigma of 0.02
 C6-C9 \\sim C29-C30
 with sigma of 0.02
 C9-C11 \\sim C30-C31
 with sigma of 0.02
 C11-C21 \\sim C31-C35
 with sigma of 0.02
 C11-C26 \\sim C31-C40
 with sigma of 0.02
 C12-C23 \\sim C32-C37
 with sigma of 0.02
 C19-C25 \\sim C33-C39
 with sigma of 0.02
 C20-C24 \\sim C34-C38
 with sigma of 0.02
 C20-C27 \\sim C34-C41
 with sigma of 0.02
 C21-C24 \\sim C35-C38
 with sigma of 0.02
 C22-C23 \\sim C36-C37
 with sigma of 0.02
 C22-C25 \\sim C36-C39
 with sigma of 0.02
 C22-C28 \\sim C36-C42
 with sigma of 0.02
 C26-C27 \\sim C40-C41
 with sigma of 0.02
 O2-O5 \\sim O2-O6
 with sigma of 0.04
 O2-C9 \\sim O2-C30
 with sigma of 0.04
 N3-C23 \\sim N5-C37
 with sigma of 0.04
 N3-C25 \\sim N5-C39
 with sigma of 0.04
 O5-C9 \\sim O6-C30
 with sigma of 0.04
 N4-C6 \\sim N6-C29
 with sigma of 0.04
 N4-C11 \\sim N6-C31
 with sigma of 0.04
 N4-C22 \\sim N6-C36
 with sigma of 0.04
 C6-C11 \\sim C29-C31
 with sigma of 0.04
 C9-C21 \\sim C30-C35
 with sigma of 0.04
 C9-C26 \\sim C30-C40
 with sigma of 0.04
 C9-C28 \\sim C30-C42
 with sigma of 0.04
 C11-C24 \\sim C31-C38
 with sigma of 0.04
 C11-C27 \\sim C31-C41
 with sigma of 0.04
 C12-C19 \\sim C32-C33
 with sigma of 0.04
 C12-C22 \\sim C32-C36
 with sigma of 0.04
 C19-C22 \\sim C33-C36
 with sigma of 0.04
 C20-C21 \\sim C34-C35
 with sigma of 0.04
 C20-C26 \\sim C34-C40
 with sigma of 0.04
 C21-C26 \\sim C35-C40
 with sigma of 0.04
 C23-C25 \\sim C37-C39
 with sigma of 0.04
 C23-C28 \\sim C37-C42
 with sigma of 0.04
 C24-C27 \\sim C38-C41
 with sigma of 0.04
 C25-C28 \\sim C39-C42
 with sigma of 0.04
 Co1-N2 \\sim Co1-N8
 with sigma of 0.02
 O1-C2 \\sim O7-C44
 with sigma of 0.02
 N2-C5 \\sim N8-C47
 with sigma of 0.02
 O4-C2 \\sim O8-C44
 with sigma of 0.02
 C1-C3 \\sim C43-C45
 with sigma of 0.02
 C2-C4 \\sim C44-C46
 with sigma of 0.02
 C3-C7 \\sim C45-C48
 with sigma of 0.02
 C3-C8 \\sim C45-C49
 with sigma of 0.02
 C4-C13 \\sim C46-C51
 with sigma of 0.02
 C5-C7 \\sim C47-C48
 with sigma of 0.02
 C13-C14 \\sim C51-C52
 with sigma of 0.02
 C13-C18 \\sim C51-C56
 with sigma of 0.02
 C14-C15 \\sim C52-C53
 with sigma of 0.02
 C17-C18 \\sim C55-C56
 with sigma of 0.02
 Co1-C5 \\sim Co1-C47
 with sigma of 0.04
 O1-O4 \\sim O7-O8
 with sigma of 0.04
 O1-C4 \\sim O7-C46
 with sigma of 0.04
 N2-C7 \\sim N8-C48
 with sigma of 0.04
 N2-C8 \\sim N8-C49
 with sigma of 0.04
 O4-C4 \\sim O8-C46
 with sigma of 0.04
 C1-C4 \\sim C43-C46
 with sigma of 0.04
 C1-C7 \\sim C43-C48
 with sigma of 0.04
 C1-C8 \\sim C43-C49
 with sigma of 0.04
 C2-C13 \\sim C44-C51
 with sigma of 0.04
 C3-C5 \\sim C45-C47
 with sigma of 0.04
 C4-C14 \\sim C46-C52
 with sigma of 0.04
 C4-C18 \\sim C46-C56
 with sigma of 0.04
 C7-C8 \\sim C48-C49
 with sigma of 0.04
 C13-C15 \\sim C51-C53
 with sigma of 0.04
 C13-C17 \\sim C51-C55
 with sigma of 0.04
 C14-C18 \\sim C52-C56
 with sigma of 0.04
 C15-C17 \\sim C53-C55
 with sigma of 0.04
 C15-C16 \\sim C53-C54
 with sigma of 0.02
 C16-C17 \\sim C54-C55
 with sigma of 0.02
 C14-C16 \\sim C52-C54
 with sigma of 0.04
 C16-C18 \\sim C54-C56
 with sigma of 0.04
 N1-C1 \\sim N7-C43
 with sigma of 0.02
 N1-C4 \\sim N7-C46
 with sigma of 0.02
 N1-C2 \\sim N7-C44
 with sigma of 0.04
 N1-C3 \\sim N7-C45
 with sigma of 0.04
 N1-C13 \\sim N7-C51
 with sigma of 0.04
 N2-C10 \\sim N8-C50
 with sigma of 0.02
 C8-C10 \\sim C49-C50
 with sigma of 0.02
 Co1-C10 \\sim Co1-C50
 with sigma of 0.04
 C3-C10 \\sim C45-C50
 with sigma of 0.04
 C5-C10 \\sim C47-C50
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C50) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 N3, O5, N4, C6, C9, C11, C12, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, O6, N6, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39, C40, C41,
 C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, N1, N2, O4, C1, C2, C3, C4, C5, C7, C8, C10, C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, N7, N8, O8, C43, C44, C45, C46, C47, C48, C49, C50, C51, C52, C53, C54,
 C55, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1(0.5) N1(0.5) H1(0.5) N2(0.5) O4(0.5) C1(0.5) H1A(0.5) H1B(0.5)
 N3(0.5) C2(0.5) O5(0.5) C3(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) N4(0.5)
 H4A(0.5) C6(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) C9(0.5) H9(0.5) C10(0.5)
 H10(0.5) C11(0.5) C12(0.5) H12(0.5) C13(0.5) C14(0.5) H14(0.5) C15(0.5)
 H15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5) C19(0.5)
 H19(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5) C22(0.5) C23(0.5) H23(0.5)
 C24(0.5) H24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5)
 C28(0.5) H28A(0.5) H28B(0.5) N5(0.5) O6(0.5) N6(0.5) H6(0.5) C29(0.5) C30(0.5)
 H30(0.5) C31(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5) C34(0.5) H34(0.5)
 C35(0.5) H35(0.5) C36(0.5) C37(0.5) H37(0.5) C38(0.5) H38(0.5) C39(0.5)
 H39(0.5) C40(0.5) H40(0.5) C41(0.5) H41(0.5) C42(0.5) H42A(0.5) H42B(0.5)
 O7(0.5) N7(0.5) H7A(0.5) N8(0.5) O8(0.5) C43(0.5) H43A(0.5) H43B(0.5) C44(0.5)
 C45(0.5) C46(0.5) H46(0.5) C47(0.5) H47(0.5) C48(0.5) H48(0.5) C49(0.5)
 H49(0.5) C50(0.5) H50(0.5) C51(0.5) C52(0.5) H52(0.5) C53(0.5) H53(0.5)
 C54(0.5) H54(0.5) C55(0.5) H55(0.5) C56(0.5) H56(0.5)
6.a Rotating group:
 O3(H3A,H3B)
6.b Ternary CH refined with riding coordinates:
 N1(H1), C4(H4), C9(H9), C30(H30), N7(H7A), C46(H46)
6.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C28(H28A,H28B), C42(H42A,H42B), C43(H43A,H43B)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), N4(H4A), C7(H7), C8(H8), C10(H10), C12(H12), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), N6(H6), C32(H32), C33(H33), C34(H34), C35(H35),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C47(H47), C48(H48), C49(H49),
  C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
6.e Fitted hexagon refined as free rotating group:
 C13(C14,C15,C16,C17,C18), C51(C52,C53,C54,C55,C56)
;
_shelx_res_checksum              29604
_shelx_hkl_checksum              7677
_olex2_submission_special_instructions 'No special instructions were received'