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_7706698
_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         'C70 H57 Cu4 N6 P4 S2, 1.25(C H2 Cl2), F6 P'
_chemical_formula_sum            'C71.25 H59.5 Cl2.5 Cu4 F6 N6 P5 S2'
_chemical_formula_weight         1675.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-02-06
_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                90
_cell_formula_units_Z            4
_cell_length_a                   13.1572(2)
_cell_length_b                   16.6001(2)
_cell_length_c                   34.5546(5)
_cell_measurement_reflns_used    20584
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      77.1820
_cell_measurement_theta_min      2.9800
_cell_volume                     7547.10(18)
_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      99.99(10)
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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   -120.00 -36.00   0.50    0.10    --  -46.81 -42.00  87.00  168
  2  \w   -125.00 -76.00   0.50    0.40    --  -88.50 -87.00-112.00   98
  3  \w    104.00 160.00   0.50    0.40    --  110.00 103.00  96.00  112
  4  \w     39.00 123.00   0.50    0.40    --  110.00 -42.00  87.00  168
  5  \w   -120.00 -72.00   0.50    0.10    --  -46.81-125.00  60.00   96
  6  \w   -115.00 -70.00   0.50    0.10    --  -46.81-125.00-120.00   90
  7  \w   -118.00 -93.00   0.50    0.10    --  -46.81-125.00  30.00   50
  8  \w   -117.00 -92.00   0.50    0.10    --  -46.81-125.00   0.00   50
  9  \w     33.00  95.00   0.50    0.10    --   46.81-125.00  30.00  124
 10  \w     58.00 125.00   0.50    0.40    --  110.00 -30.00 -90.00  134
 11  \w     58.00  85.00   0.50    0.40    --  110.00 -94.00  90.00   54
 12  \w     40.00  83.00   0.50    0.40    --  110.00-125.00 -60.00   86
 13  \w    121.00 148.00   0.50    0.40    --  110.00  87.00   5.00   54
 14  \w     39.00 100.00   0.50    0.40    --  110.00-125.00   0.00  122
 15  \w     96.00 175.00   0.50    0.40    --  110.00  45.00 -90.00  158
 16  \w     39.00 128.00   0.50    0.40    --  110.00 -61.00 -30.00  178
;
_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  0.0506
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            43339
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.032
_diffrn_reflns_theta_min         2.953
_exptl_absorpt_coefficient_mu    4.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47203
_exptl_absorpt_correction_type   integration
_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    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             3394
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.063
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Flack x determined using 5733 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         15446
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0952P)^2^+12.8730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                14130
_reflns_number_total             15446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00031d3.cif
_cod_data_source_block           2e-m
_cod_depositor_comments
'Adding full bibliography for 7706697--7706707.cif.'
_cod_original_formula_sum        'C71.25 H59.50 Cl2.50 Cu4 F6 N6 P5 S2'
_cod_database_code               7706698
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.495
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl3-C70
 1.73 with sigma of 0.02
 C70-Cl4
 1.73 with sigma of 0.02
 Cu4-H \\sim Cu3-H \\sim Cu2-H \\sim Cu1-H
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl3) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C69) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(H) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl3(0.25) Cl4(0.25) C70(0.25) H70A(0.25) H70B(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70(H70A,H70B)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C53(H53), C64(H64), C61(H61), C47(H47), C38(H38), C11(H11),
 C20(H20), C60(H60), C2(H2), C30(H30), C59(H59), C51(H51), C41(H41), C57(H57),
 C33(H33), C10(H10), C54(H54), C65(H65), C58(H58), C4(H4), C48(H48), C19(H19),
 C55(H55), C68(H68), C44(H44), C13(H13), C1(H1), C37(H37), C9(H9), C43(H43),
 C67(H67), C26(H26), C7(H7), C34(H34), C32(H32), C18(H18), C42(H42), C49(H49),
 C66(H66), C45(H45), C14(H14), C31(H31), C8(H8), C27(H27), C24(H24), C25(H25),
 C36(H36), C35(H35), C50(H50), C56(H56), C3(H3), C15(H15), C28(H28), C16(H16),
 C17(H17)
;
_shelx_res_checksum              8635
_shelx_hkl_checksum              20518
_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
;