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_7706703
_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, F6 P, 1.25(C H2 Cl2)'
_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                   13.1571(2)
_cell_length_b                   16.5948(2)
_cell_length_c                   34.5954(4)
_cell_measurement_reflns_used    33179
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.7460
_cell_measurement_theta_min      2.9710
_cell_volume                     7553.54(17)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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  0.0478
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            46245
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.958
_diffrn_reflns_theta_min         4.222
_exptl_absorpt_coefficient_mu    4.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38953
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       clear
_exptl_crystal_F_000             3394
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 6107 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         15033
_refine_ls_number_restraints     614
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0506P)^2^+9.6745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.915
_reflns_number_gt                14485
_reflns_number_total             15033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00031d3.cif
_cod_data_source_block           2e-p
_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               7706703
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.373
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl3-C72 = Cl4-C72
 1.73 with sigma of 0.02
 Cu3-H \\sim Cu2-H \\sim Cu1-H \\sim Cu4-H
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C72) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(H) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Cl4(0.25) Cl3(0.25) C72(0.25) H72A(0.25) H72B(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B)
5.b Aromatic/amide H refined with riding coordinates:
 C61(H61), C65(H65), C38(H38), C44(H44), C40(H40), C42(H42), C47(H47),
 C37(H37), C4(H4), C21(H21), C13(H13), C54(H54), C55(H55), C41(H41), C30(H30),
 C26(H26), C33(H33), C9(H9), C68(H68), C63(H63), C60(H60), C7(H7), C52(H52),
 C19(H19), C10(H10), C66(H66), C59(H59), C48(H48), C51(H51), C57(H57), C34(H34),
  C31(H31), C5(H5), C43(H43), C20(H20), C18(H18), C53(H53), C14(H14), C67(H67),
 C11(H11), C50(H50), C49(H49), C32(H32), C2(H2), C36(H36), C8(H8), C28(H28),
 C25(H25), C58(H58), C35(H35), C3(H3), C27(H27), C24(H24), C15(H15), C17(H17),
 C16(H16)
;
_shelx_res_checksum              27664
_shelx_hkl_checksum              62743
_olex2_submission_special_instructions 'No special instructions were received'