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_7706706
_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, 0.667(C3 H6 Br6)'
_chemical_formula_sum            'C53 H47 Br7 Cu4 N3 P3'
_chemical_formula_weight         1632.37
_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                   14.9752(2)
_cell_length_b                   14.9752(2)
_cell_length_c                   22.1086(2)
_cell_measurement_reflns_used    24572
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.9400
_cell_measurement_theta_min      3.9320
_cell_volume                     4293.75(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -27.00  62.00   0.50    1.52    --   46.75 -37.00 -90.00  178
  2  \w     31.00  96.00   0.50    1.52    --   46.75-125.00-120.00  130
  3  \w     38.00 117.00   0.50    6.20    --  110.00-125.00-180.00  158
  4  \w     38.00 109.00   0.50    6.20    --  110.00 -94.00 -90.00  142
  5  \w     35.00 128.00   0.50    6.20    --  110.00 -15.00-180.00  186
  6  \w     96.00 178.00   0.50    6.20    --  110.00  45.00 -60.00  164
  7  \w     96.00 178.00   0.50    6.20    --  110.00  30.00   0.00  164
  8  \w     93.00 178.00   0.50    6.20    --  110.00  61.00  90.00  170
  9  \w     87.00 178.00   0.50    6.20    --  110.00  76.00  65.54  182
 10  \w     38.00 125.00   0.50    6.20    --  110.00 -45.00  90.00  174
 11  \w     38.00 117.00   0.50    6.20    --  110.00-125.00  90.00  158
 12  \w     38.00 109.00   0.50    6.20    --  110.00 -94.00 -30.00  142
 13  \w     38.00 117.00   0.50    6.20    --  110.00-125.00 -90.00  158
 14  \w     38.00 117.00   0.50    6.20    --  110.00-125.00-120.00  158
 15  \w     38.00 134.00   0.50    6.20    --  110.00 -77.00  30.00  192
 16  \w     38.00 134.00   0.50    6.20    --  110.00 -77.00-150.00  192
 17  \w     37.00 178.00   0.50    6.20    --  110.00   0.00 -90.00  282
 18  \w     38.00 109.00   0.50    6.20    --  110.00 -94.00  30.00  142
 19  \w     38.00 128.00   0.50    6.20    --  110.00 -61.00 -90.00  180
 20  \w     35.00 128.00   0.50    6.20    --  110.00 -15.00 -90.00  186
 21  \w     38.00 128.00   0.50    6.20    --  110.00 -61.00  90.00  180
 22  \w     -4.00  81.00   0.50    1.52    --   46.75 -99.00-120.00  170
 23  \w     -4.00  81.00   0.50    1.52    --   46.75 -99.00 -90.00  170
 24  \w    -62.00  29.00   0.50    1.52    --  -46.75  19.00 120.00  182
 25  \w   -103.00 -16.00   0.50    6.20    --  -88.50  45.00 150.00  174
 26  \w   -119.00 -23.00   0.50    1.52    --  -46.75 -77.00 -60.00  192
 27  \w   -119.00 -70.00   0.50    1.52    --  -46.75-125.00   0.00   98
 28  \w   -119.00 -70.00   0.50    1.52    --  -46.75-125.00-120.00   98
 29  \w   -119.00 -70.00   0.50    1.52    --  -46.75-125.00 -90.00   98
 30  \w   -119.00 -30.00   0.50    1.52    --  -46.75 -57.00-150.00  178
 31  \w   -119.00 -70.00   0.50    1.52    --  -46.75-125.00  30.00   98
 32  \w   -119.00 -23.00   0.50    1.52    --  -46.75 -77.00  30.00  192
 33  \w   -119.00 -30.00   0.50    1.52    --  -46.75 -57.00 -60.00  178
 34  \w   -119.00 -30.00   0.50    1.52    --  -46.75 -57.00  60.00  178
 35  \w   -119.00 -23.00   0.50    1.52    --  -46.75 -77.00 150.00  192
 36  \w   -160.00 -69.00   0.50    6.20    --  -88.50 -83.00-133.50  182
 37  \w   -160.00 -62.00   0.50    6.20    --  -88.50 -82.00  -3.01  196
 38  \w   -160.00 -65.00   0.50    6.20    --  -88.50 -77.00 120.00  190
 39  \w   -160.00 -66.00   0.50    6.20    --  -88.50 -74.00 178.84  188
 40  \w   -160.00 -65.00   0.50    6.20    --  -88.50 -77.00  60.00  190
 41  \w   -160.00 -65.00   0.50    6.20    --  -88.50 -76.00-100.13  190
;
_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  0.0446
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34208
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.700
_diffrn_reflns_theta_max         78.290
_diffrn_reflns_theta_min         3.952
_exptl_absorpt_coefficient_mu    8.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 1870 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4056
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0412P)^2^+16.4584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.981
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                3944
_reflns_number_total             4056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00031d3.cif
_cod_data_source_block           3b-delta-ch2br2
_cod_depositor_comments
'Adding full bibliography for 7706697--7706707.cif.'
_cod_original_cell_volume        4293.75(12)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7706706
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.484
_shelx_estimated_absorpt_t_min   0.484
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Br2(0.33333) H19A(0.33333) H19B(0.33333) Br3(0.33333) Br4(0.33333)
 Br5(0.33333) C18(0.33333) H4A(0.33333) H4B(0.33333)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H4A,H4B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17)
;
_shelx_res_checksum              21869
_shelx_hkl_checksum              83112
_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
;