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_7706701
_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         'C68 H57 Cu4 I2 N4 P4, F6 P, C H2 Cl2'
_chemical_formula_sum            'C69 H59 Cl2 Cu4 F6 I2 N4 P5'
_chemical_formula_weight         1791.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 92.5280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.42630(10)
_cell_length_b                   12.03160(10)
_cell_length_c                   35.2262(3)
_cell_measurement_reflns_used    25472
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.0500
_cell_measurement_theta_min      2.9170
_cell_volume                     6955.14(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.21a (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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.953
_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    -86.00  -6.00   0.50    0.10    --  -46.81 113.00 171.00  160
  2  \w     34.00  60.00   0.50    0.10    --   46.81-113.00  79.00   52
  3  \w   -119.00 -78.00   0.50    0.40    --  -88.50-113.00  79.00   82
  4  \w    -76.00 -50.00   0.50    0.40    --  -88.50 113.00 171.00   52
  5  \w     33.00 107.00   0.50    0.40    --  105.73-113.00  79.00  148
  6  \w    112.00 137.00   0.50    0.40    --  105.73 113.00 171.00   50
  7  \w   -109.00 -71.00   0.50    0.10    --  -46.81-125.00-120.00   76
  8  \w   -114.00 -88.00   0.50    0.10    --  -46.81-125.00 -90.00   52
  9  \w    -60.00  27.00   0.50    0.10    --  -46.81  19.00  90.00  174
 10  \w   -114.00 -77.00   0.50    0.10    --  -46.81-125.00-150.00   74
 11  \w   -160.00-130.00   0.50    0.40    --  -88.50 -94.00-150.00   60
 12  \w   -138.00-112.00   0.50    0.40    --  -88.50 -94.00 -90.00   52
 13  \w   -101.00 -74.00   0.50    0.40    --  -88.50 -45.00 120.00   54
 14  \w   -110.00 -81.00   0.50    0.40    --  -88.50 -94.00-150.00   58
 15  \w   -161.00-117.00   0.50    0.40    --  -88.50 -45.00 120.00   88
 16  \w     39.00  73.00   0.50    0.40    --  105.73 -94.00 120.00   68
 17  \w    150.00 178.00   0.50    0.40    --  105.73  45.00-120.00   56
 18  \w     92.00 142.00   0.50    0.40    --  105.73  45.00-120.00  100
 19  \w     33.00 114.00   0.50    0.40    --  105.73-125.00 -90.00  162
 20  \w     92.00 146.00   0.50    0.40    --  105.73 125.00 -90.00  108
 21  \w     35.00 107.00   0.50    0.40    --  105.73 -94.00 -60.00  144
 22  \w     88.00 160.00   0.50    0.40    --  105.73  77.00  60.00  144
 23  \w     78.00 105.00   0.50    0.40    --  105.73 -94.00 120.00   54
;
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            49484
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.941
_diffrn_reflns_theta_min         2.921
_exptl_absorpt_coefficient_mu    10.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.21a (Rigaku Oxford Diffraction, 2018)
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    1.711
_exptl_crystal_description       block
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.010
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         13832
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0391P)^2^+10.9395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12826
_reflns_number_total             13832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00031d3.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 7706697--7706707.cif.'
_cod_database_code               7706701
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.416
_shelx_estimated_absorpt_t_min   0.225
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cu1-H \\sim Cu2-H \\sim Cu4-H \\sim Cu3-H
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(H) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B)
4.b Aromatic/amide H refined with riding coordinates:
 C64(H64), C51(H51), C19(H19), C20(H20), C26(H26), C2(H2), C5(H5), C4(H4),
 C23(H23), C53(H53), C16(H16), C50(H50), C68(H68), C56(H56), C24(H24), C65(H65),
  C39(H39), C48(H48), C54(H54), C62(H62), C49(H49), C59(H59), C25(H25),
 C22(H22), C21(H21), C47(H47), C7(H7), C15(H15), C29(H29), C11(H11), C66(H66),
 C3(H3), C60(H60), C55(H55), C43(H43), C12(H12), C30(H30), C10(H10), C13(H13),
 C61(H61), C41(H41), C67(H67), C8(H8), C9(H9), C45(H45), C58(H58), C33(H33),
 C14(H14), C35(H35), C44(H44), C31(H31), C42(H42), C32(H32), C36(H36), C38(H38),
  C37(H37)
;
_shelx_res_checksum              74425
_shelx_hkl_checksum              7784
_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
;