Modulating the ferroelectric performance by altering halogen anions in the crystals of tetranuclear copper-clusters
Liu, Meiying; Liang, Jingjing; Liu, Zhiliang; New Journal of Chemistry 45 (2021) 12091–12096; doi:10.1039/D1NJ01894A

data_7060710
_publ_section_title
;
 Modulating the ferroelectric performance by altering halogen anions in
 the crystals of tetranuclear copper-clusters
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12091
_journal_page_last               12096
_journal_paper_doi               10.1039/D1NJ01894A
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C70 H76 Cu4 N4 O14, 2(Cl)'
_chemical_formula_sum            'C70 H76 Cl2 Cu4 N4 O14'
_chemical_formula_weight         1522.40
_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
_audit_creation_date             2021-05-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-05-31 deposited with the CCDC.	2021-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.173(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4998(19)
_cell_length_b                   25.108(5)
_cell_length_c                   15.766(3)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.74
_cell_volume                     3925.8(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            88529
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.200
_diffrn_reflns_theta_min         2.736
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0736 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.8363.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.320
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details
;
 Flack x determined using 5308 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.250(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         13976
_refine_ls_number_restraints     565
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.1099
_refine_ls_shift/su_max          1.565
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1919P)^2^+24.1186P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2856
_refine_ls_wR_factor_ref         0.2966
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                12472
_reflns_number_total             13976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01894a2.cif
_cod_data_source_block           a-auto_sq
_cod_depositor_comments
'Adding full bibliography for 7060709--7060710.cif.'
_cod_database_code               7060710
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.726(5)
 0.274(5)
2. 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, All O(H) groups
3. Restrained distances
 O3-H3A
 0.85 with sigma of 0.01
 O14-H14A
 0.85 with sigma of 0.01
 O12-H12
 0.85 with sigma of 0.01
 O13-H13A
 0.85 with sigma of 0.01
 C69-H13A
 1.895333 with sigma of 0.02
 C10-H3A
 1.942632 with sigma of 0.02
 Cu4-H14A
 2.816853 with sigma of 0.02
 Cu1-H13A
 2.742086 with sigma of 0.02
 C61-H12
 1.905578 with sigma of 0.02
 Cu1-H3A
 2.697021 with sigma of 0.02
 Cu4-H12
 2.683382 with sigma of 0.02
 C70-H14A
 1.892784 with sigma of 0.02
4. Rigid bond restraints
 O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
6.a Ternary CH refined with riding coordinates:
 C43(H43), C9(H9), C60(H60), C26(H26)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C45(H45A,H45B), C10(H10A,H10B), C62(H62A,
 H62B), C61(H61A,H61B)
6.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C25(H25), C30(H30), C33(H33), C34(H34),
 C37(H37), C38(H38), C39(H39), C42(H42), C44(H44), C51(H51), C50(H50), C49(H49),
  C48(H48), C47(H47), C13(H13), C17(H17), C16(H16), C15(H15), C14(H14),
 C11(H11), C8(H8), C5(H5), C4(H4), C3(H3), C66(H66), C65(H65), C64(H64),
 C68(H68), C67(H67), C59(H59), C31(H31), C32(H32), C56(H56), C55(H55), C54(H54)
6.d Fitted hexagon refined as free rotating group:
 C13(C12,C17,C16,C15,C14), C66(C65,C64,C63,C68,C67)
6.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C35(H35A,H35B,H35C), C1(H1A,H1B,H1C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              80681
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_fab_checksum              2134