Chiral zero-dimensional hybrid organic–inorganic metal halides based on nipecotic acid and tetrabromocuprate
Wang, Xianran; Wu, Yuying; Gao, Feng; Wang, Youfu; New Journal of Chemistry 48 (2024) 3192–3198; doi:10.1039/D3NJ05858A

data_7062959
_publ_section_title
;
 Chiral zero-dimensional hybrid organic--inorganic metal halides based on
 nipecotic acid and tetrabromocuprate
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3192
_journal_page_last               3198
_journal_paper_doi               10.1039/D3NJ05858A
_journal_volume                  48
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Br4 Cu1, 2(C6 H12 N O2)'
_chemical_formula_sum            'C12 H24 Br4 Cu N2 O4'
_chemical_formula_weight         643.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-06 deposited with the CCDC.	2024-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3889(5)
_cell_length_b                   9.8846(7)
_cell_length_c                   25.0684(17)
_cell_measurement_reflns_used    7357
_cell_measurement_temperature    296.00
_cell_measurement_theta_max      68.331
_cell_measurement_theta_min      6.923
_cell_volume                     2078.7(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SMART APEX II diffractometer'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.00
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15127
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.326
_diffrn_reflns_theta_min         6.923
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           45.0
_diffrn_source_power             2.25
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.646
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0884 before and 0.0776 after correction.
The Ratio of minimum to maximum transmission is 0.8308.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1902
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+2.3505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1763
_reflns_number_total             1902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj05858a2.cif
_cod_data_source_block           '[s-na]2[cubr4]'
_cod_depositor_comments
'Adding full bibliography for 7062959--7062960.cif.'
_cod_database_code               7062959
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.416
_shelx_estimated_absorpt_t_min   0.281
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.92(5)
 0.08(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Uiso/Uaniso restraints and constraints
Cu1 \\sim Cu2 \\sim Cu3 \\sim Cu4 \\sim Br5 \\sim Br1 \\sim Br4 \\sim Br2 \\sim
Br3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
4. Others
 1*[Sof(Br1)]+1*[Sof(Br4)]+1*[Sof(Br2)]+1*[Sof(Br3)]=1 with esd of 0.0001
 1*[Sof(Cu1)]+1*[Sof(Cu2)]+1*[Sof(Cu3)]+1*[Sof(Cu4)]=0.5 with esd of 0.0001
 Sof(H2A)=1-FVAR(7)
 Sof(H1)=FVAR(7)
5.a Ternary CH refined with riding coordinates:
 C2(H2)
5.b Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), C6(H6A,H6B), C3(H3A,H3B), C4(H4C,H4D), C5(H5A,H5B)
5.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2A)
;
_shelx_res_checksum              69112
_olex2_submission_special_instructions 'No special instructions were received'