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_7706700
_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 Cl2 Cu4 N4 P4, 2(C H2 Cl2), F6 P'
_chemical_formula_sum            'C70 H61 Cl6 Cu4 F6 N4 P5'
_chemical_formula_weight         1693.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 96.2320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.70320(10)
_cell_length_b                   26.1636(2)
_cell_length_c                   20.0973(2)
_cell_measurement_reflns_used    21676
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.9720
_cell_measurement_theta_min      4.0360
_cell_volume                     7162.81(10)
_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
'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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   -123.00 -43.00   1.00    0.21    --  -46.62 -23.00 104.00   80
  2  \w     55.00  83.00   1.00    0.21    --   46.62  23.00 -91.00   28
  3  \w     -8.00  17.00   1.00    0.21    --   46.62 -23.00 104.00   25
  4  \w   -116.00 -90.00   1.00    0.84    --  -88.50 -23.00 104.00   26
  5  \w   -102.00 -54.00   1.00    0.84    --  -88.50  23.00 -91.00   48
  6  \w     96.00 177.00   1.00    0.84    --  110.00  23.00 -91.00   81
  7  \w     79.00 112.00   1.00    0.84    --  110.00 -23.00 104.00   33
  8  \w     36.00  61.00   1.00    0.84    --  110.00 -23.00 104.00   25
  9  \w    -58.00  27.00   1.00    0.21    --  -46.62  37.00 -30.00   85
 10  \w    -58.00  29.00   1.00    0.21    --  -46.62  23.00 -91.00   87
 11  \w     59.00  86.00   1.00    0.21    --   46.62-125.00 -60.00   27
 12  \w    -90.00 -21.00   1.00    0.84    --  -88.50 125.00-120.00   69
 13  \w     41.00 104.00   1.00    0.84    --  110.00 -94.00 -90.00   63
 14  \w     92.00 178.00   1.00    0.84    --  110.00  15.00-150.00   86
 15  \w     40.00 107.00   1.00    0.84    --  110.00 -94.00-180.00   67
 16  \w     42.00  84.00   1.00    0.84    --  110.00 -45.00  30.00   42
 17  \w     41.00  91.00   1.00    0.84    --  110.00 -94.00 120.00   50
 18  \w     94.00 124.00   1.00    0.84    --  110.00 -45.00  30.00   30
 19  \w     42.00 109.00   1.00    0.84    --  110.00 -94.00   0.00   67
 20  \w     98.00 128.00   1.00    0.84    --  110.00 -77.00-180.00   30
 21  \w     52.00  90.00   1.00    0.84    --  110.00 -77.00-180.00   38
 22  \w     84.00 109.00   1.00    0.84    --  110.00 -94.00  60.00   25
;
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53513
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.166
_diffrn_reflns_theta_min         3.658
_exptl_absorpt_coefficient_mu    4.955
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49869
_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.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         14835
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0400P)^2^+9.3361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12352
_reflns_number_total             14835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00031d3.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7706697--7706707.cif.'
_cod_original_cell_volume        7162.80(10)
_cod_database_code               7706700
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.437
_shelx_estimated_absorpt_t_min   0.437
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(H) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H71C)=Sof(H71D)=Sof(Cl4B)=1-FVAR(1)
 Sof(H71A)=Sof(H71B)=Sof(Cl4A)=FVAR(1)
 Sof(Cl5A)=Sof(Cl6B)=Sof(C70)=Sof(H70A)=Sof(H70B)=1-FVAR(2)
 Sof(Cl5B)=Sof(Cl6A)=Sof(C69)=Sof(H69A)=Sof(H69B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C71(H71C,H71D), C71(H71A,H71B), C70(H70A,H70B), C69(H69A,H69B)
4.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), C18(H18), C19(H19), C20(H20),
  C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66),
 C67(H67), C68(H68)
;
_shelx_res_checksum              80900
_shelx_hkl_checksum              6866
_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
;