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_7060709
_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         'C68.712 H75.424 Cu4 N4 O14, 2(Br)'
_chemical_formula_sum            'C68.71 H75.43 Br2 Cu4 N4 O14'
_chemical_formula_weight         1595.25
_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             2021-05-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-05-17 deposited with the CCDC.	2021-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.987(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2904(5)
_cell_length_b                   21.3262(9)
_cell_length_c                   15.8441(7)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.22
_cell_measurement_theta_min      2.98
_cell_volume                     3468.7(3)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            86122
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.749
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.427
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6234
_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    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             1627
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 5043 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         12882
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0311P)^2^+1.2355P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                11288
_reflns_number_total             12882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01894a2.cif
_cod_data_source_block           mo_171017e_0m
_cod_depositor_comments
'Adding full bibliography for 7060709--7060710.cif.'
_cod_database_code               7060709
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.811
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9
 0.85 with sigma of 0.01
 O3-H3A
 0.85 with sigma of 0.01
 O13B-H13B
 0.85 with sigma of 0.01
 O13A-H13C = O13A-H13A
 0.85 with sigma of 0.02
 H13A-O5
 1 with sigma of 0.1
 C17-H9
 1.922206 with sigma of 0.02
 Cu1-H9
 2.731233 with sigma of 0.02
 C68-H3A
 1.933862 with sigma of 0.02
 Cu4-H3A
 2.683168 with sigma of 0.02
 Cu4-H13B
 2.655452 with sigma of 0.02
 C69-H13B
 1.847995 with sigma of 0.02
 H13C-H13A
 1.34 with sigma of 0.04
 Cu4-H13C \\sim Cu4-H13A
 with sigma of 0.02
3. Rigid bond restraints
 O13B, C69
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
4. Others
 Sof(Br3)=Sof(Br4)=Sof(O13A)=Sof(H13A)=Sof(H13C)=1-FVAR(1)
 Sof(Br2)=Sof(Br1)=Sof(O13B)=Sof(H13B)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=
 FVAR(1)
5.a Riding coordinates:
 O13A(H13A,H13C)
5.b Rotating group:
 O14(H14A,H14B)
5.c Ternary CH refined with riding coordinates:
 C33(H33), C16(H16), C50(H50), C67(H67)
5.d Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C15(H15A,H15B), C51(H51A,H51B), C17(H17A,H17B), C34(H34A,
 H34B), C66(H66A,H66B), C49(H49A,H49B), C68(H68A,H68B)
5.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C25(H25), C5(H5), C4(H4), C39(H39), C22(H22), C44(H44),
 C55(H55), C56(H56), C42(H42), C21(H21), C54(H54), C47(H47), C45(H45), C26(H26),
  C43(H43), C20(H20), C37(H37), C12(H12), C9(H9A), C38(H38), C13(H13), C46(H46),
  C64(H64), C60(H60), C61(H61), C30(H30), C11(H11), C62(H62), C10(H10),
 C29(H29), C63(H63), C59(H59), C27(H27), C28(H28)
5.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C52(H52A,H52B,H52C), C35(H35A,H35B,
 H35C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              73116
_olex2_submission_special_instructions 'No special instructions were received'