Dissection of bicapped octahedral copper hydride cluster to form two chiral tetrahedral copper hydride cluster series exhibiting auto deracemization and photoluminescence.
Xu, Han; Han, Ying-Zi; OuYang, Jie; Chen, Zuo-Chang; Chen, Hui-Jun; Nie, Hong-Hong; Tang, Zichao; Yang, Shi-Yao; Huang, Rong-Bin; Zheng, Lan-Sun; Teo, Boon K.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4028–4035; doi:10.1039/d1dt00031d

data_7706704
_publ_section_title
;
 Dissection of bicapped octahedral copper hydride cluster to form two
 chiral tetrahedral copper hydride cluster series exhibiting auto
 deracemization and photoluminescence.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4028
_journal_page_last               4035
_journal_paper_doi               10.1039/d1dt00031d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C51 H43 Br3 Cu4 N3 P3, 2(C1 H2 Cl2)'
_chemical_formula_sum            'C53 H47 Br3 Cl4 Cu4 N3 P3'
_chemical_formula_weight         1454.53
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-01-24
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.05.22 svn.r3605 for OlexSys, GUI svn.r5790)
;
_audit_update_record
;
2021-02-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.7989(2)
_cell_length_b                   14.7989(2)
_cell_length_c                   22.1361(3)
_cell_measurement_reflns_used    8509
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2130
_cell_measurement_theta_min      3.9800
_cell_volume                     4198.47(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -129.00 -74.00   0.50    0.80    --  -88.50 -29.00  54.00  110
  2  \w   -164.00 -85.00   0.50    0.80    --  -88.50 -14.00 109.00  158
  3  \w     94.00 133.00   0.50    0.80    --  107.94 -82.00-140.00   78
  4  \w     95.00 173.00   0.50    0.80    --  107.94  29.00-144.00  156
  5  \w     64.00  91.00   0.50    0.80    --  107.94 -82.00-140.00   54
  6  \w   -120.00 -80.00   0.50    0.20    --  -46.87-125.00 -60.00   80
  7  \w   -117.00 -80.00   0.50    0.20    --  -46.87 -77.00-120.00   74
  8  \w   -105.00 -80.00   0.50    0.20    --  -46.87-125.00 150.00   50
  9  \w   -121.00 -46.00   0.50    0.20    --  -46.87 -37.00 -30.00  150
 10  \w    -99.00 -70.00   0.50    0.20    --  -46.87-125.00   0.00   58
 11  \w    -76.00 -39.00   0.50    0.20    --  -46.87 -77.00-120.00   74
 12  \w     25.00  79.00   0.50    0.20    --   46.87-112.00 -29.00  108
 13  \w   -114.00 -78.00   0.50    0.80    --  -88.50 -61.00 -90.00   72
 14  \w    -78.00 -29.00   0.50    0.80    --  -88.50 112.00  63.00   98
 15  \w    152.00 178.00   0.50    0.80    --  107.94  45.00 -30.00   52
 16  \w    100.00 177.00   0.50    0.80    --  107.94  45.00-120.00  154
 17  \w     98.00 146.00   0.50    0.80    --  107.94  45.00 -30.00   96
 18  \w     76.00 109.00   0.50    0.80    --  107.94 -61.00  60.00   66
 19  \w     40.00  75.00   0.50    0.80    --  107.94 -94.00-150.00   70
 20  \w     37.00 117.00   0.50    0.80    --  107.94-125.00 -60.00  160
 21  \w     57.00 125.00   0.50    0.80    --  107.94 -61.00 -30.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10086
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.678
_diffrn_reflns_theta_min         3.986
_exptl_absorpt_coefficient_mu    7.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 1701 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3703
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+23.0689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                3627
_reflns_number_total             3703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00031d3.cif
_cod_data_source_block           3b-lamuda-ch2cl2
_cod_depositor_comments
'Adding full bibliography for 7706697--7706707.cif.'
_cod_original_cell_volume        4198.46(13)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7706704
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.331
_shelx_estimated_absorpt_t_min   0.331
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Cl1(0.66667) H18A(0.33333) H18B(0.33333) Cl2(0.33333) Cl3(0.33333)
 C19(0.33333) H19A(0.33333) H19B(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17)
;
_shelx_res_checksum              41833
_shelx_hkl_checksum              2631
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;