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_7706702
_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 N10 P4, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C70 H61 Cl4 Cu4 F6 N10 P5'
_chemical_formula_weight         1707.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                 121.0420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.2978(2)
_cell_length_b                   18.41230(10)
_cell_length_c                   15.20620(10)
_cell_measurement_reflns_used    75047
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      76.9740
_cell_measurement_theta_min      2.9350
_cell_volume                     7267.98(11)
_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      100.15
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_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     12.00  63.00   0.50    0.20    --   46.81 -57.00 -30.00  102
  2  \w     29.00  57.00   0.50    0.20    --   46.81-113.00 -40.00   56
  3  \w     31.00  96.00   0.50    0.20    --   46.81-125.00-120.00  130
  4  \w     75.00 110.00   0.50    0.80    --  108.56-113.00 -40.00   70
  5  \w    103.00 128.00   0.50    0.80    --  108.56 -77.00 -90.00   50
  6  \w     51.00  90.00   0.50    0.80    --  108.56 -61.00-180.00   78
  7  \w     37.00  76.00   0.50    0.80    --  108.56 -77.00 -90.00   78
  8  \w     39.00 106.00   0.50    0.80    --  108.56 -94.00 -30.00  134
  9  \w     40.00 107.00   0.50    0.80    --  108.56 -94.00  60.00  134
 10  \w     36.00 132.00   0.50    0.80    --  108.56 -77.00  60.00  192
 11  \w     37.00 105.00   0.50    0.80    --  108.56-125.00 -90.00  136
 12  \w     32.00  65.00   0.50    0.20    --   46.81  37.00 120.00   66
 13  \w     32.00  60.00   0.50    0.20    --   46.81  57.00 150.00   56
 14  \w     33.00  94.00   0.50    0.20    --   46.81  37.00  60.00  122
 15  \w     99.00 168.00   0.50    0.80    --  108.56 113.00  51.00  138
 16  \w     92.00 173.00   0.50    0.80    --  108.56 125.00 -60.00  162
 17  \w    107.00 178.00   0.50    0.80    --  108.56  45.00-180.00  142
 18  \w     32.00  74.00   0.50    0.20    --   46.81  37.00 -60.00   84
 19  \w     31.00  64.00   0.50    0.20    --   46.81  57.00 -90.00   66
 20  \w     36.00 101.00   0.50    0.20    --   46.81  37.00-180.00  130
 21  \w    -54.00 -15.00   0.50    0.80    --  -88.50 113.00  51.00   78
 22  \w    -84.00  -3.00   0.50    0.20    --  -46.81 113.00  51.00  162
 23  \w     36.00 108.00   0.50    0.80    --  108.56 -94.00 150.00  144
 24  \w    -61.00 -23.00   0.50    0.20    --  -46.81 -77.00-180.00   76
 25  \w    -75.00 -23.00   0.50    0.20    --  -46.81 -77.00 -90.00  104
 26  \w    -79.00 -23.00   0.50    0.20    --  -46.81 -77.00 -30.00  112
 27  \w    -78.00 -23.00   0.50    0.20    --  -46.81 -77.00   0.00  110
 28  \w    -66.00 -24.00   0.50    0.20    --  -46.81 -77.00 120.00   84
 29  \w    -68.00 -25.00   0.50    0.20    --  -46.81 -77.00 150.00   86
 30  \w    -93.00 -23.00   0.50    0.20    --  -46.81 -77.00  60.00  140
 31  \w    -90.00 -65.00   0.50    0.80    --  -88.50 -76.00  83.15   50
 32  \w    -94.00 -65.00   0.50    0.80    --  -88.50 -77.00  60.00   58
 33  \w    -91.00 -65.00   0.50    0.80    --  -88.50 -76.00   8.75   52
 34  \w    -91.00 -65.00   0.50    0.80    --  -88.50 -79.00 -16.52   52
 35  \w    -91.00 -66.00   0.50    0.80    --  -88.50 -74.00 -56.84   50
 36  \w    -97.00 -62.00   0.50    0.80    --  -88.50 -82.00  -6.31   70
 37  \w    -88.00 -63.00   0.50    0.80    --  -88.50 -81.00  27.19   50
 38  \w    -94.00 -63.00   0.50    0.80    --  -88.50 -83.00 114.21   62
 39  \w   -120.00 -87.00   0.50    0.20    --  -46.81 -77.00 120.00   66
 40  \w   -113.00 -63.00   0.50    0.80    --  -88.50 -80.00 130.22  100
 41  \w   -119.00 -93.00   0.50    0.80    --  -88.50 -76.00  83.15   52
 42  \w   -112.00 -64.00   0.50    0.80    --  -88.50 -79.00  71.67   96
 43  \w   -109.00 -82.00   0.50    0.80    --  -88.50-113.00 -40.00   54
 44  \w   -113.00 -65.00   0.50    0.80    --  -88.50 -77.00   0.00   96
 45  \w    -98.00 -62.00   0.50    0.80    --  -88.50 -82.00 -63.28   72
 46  \w    -90.00 -65.00   0.50    0.80    --  -88.50 -77.00 -90.00   50
 47  \w    -88.00 -63.00   0.50    0.80    --  -88.50 -81.00 -98.25   50
 48  \w    -92.00 -62.00   0.50    0.80    --  -88.50 -82.00-159.73   60
 49  \w    -84.00 -23.00   0.50    0.20    --  -46.81 -77.00-120.00  122
 50  \w    -99.00 -72.00   0.50    0.80    --  -88.50 -64.00 -59.64   54
 51  \w   -112.00 -86.00   0.50    0.20    --  -46.81 -77.00 -90.00   52
 52  \w   -117.00 -82.00   0.50    0.20    --  -46.81 -77.00 -30.00   70
 53  \w   -117.00 -68.00   0.50    0.80    --  -88.50 -68.00 -90.04   98
 54  \w    -98.00 -65.00   0.50    0.80    --  -88.50 -77.00-150.00   66
 55  \w   -101.00 -64.00   0.50    0.80    --  -88.50 -79.00-123.64   74
 56  \w   -117.00 -91.00   0.50    0.20    --  -46.81 -77.00-180.00   52
 57  \w   -111.00 -68.00   0.50    0.80    --  -88.50 -71.00-150.40   86
 58  \w   -116.00 -65.00   0.50    0.80    --  -88.50 -77.00-180.00  102
 59  \w   -140.00-106.00   0.50    0.80    --  -88.50 -77.00 -90.00   68
 60  \w   -147.00-100.00   0.50    0.80    --  -88.50 -79.00 -16.52   94
 61  \w   -138.00 -66.00   0.50    0.80    --  -88.50 -74.00  40.65  144
 62  \w   -135.00 -63.00   0.50    0.80    --  -88.50 -80.00  95.99  144
 63  \w   -137.00 -63.00   0.50    0.80    --  -88.50 -80.00 146.12  148
 64  \w   -140.00-115.00   0.50    0.80    --  -88.50 -79.00  71.67   50
 65  \w   -154.00-106.00   0.50    0.80    --  -88.50 -77.00  60.00   96
 66  \w   -152.00 -65.00   0.50    0.80    --  -88.50 -77.00  30.00  174
 67  \w   -148.00-123.00   0.50    0.80    --  -88.50 -79.00-123.64   50
 68  \w   -147.00-115.00   0.50    0.80    --  -88.50 -82.00 -63.28   64
 69  \w   -154.00-113.00   0.50    0.80    --  -88.50 -74.00 -56.84   82
 70  \w   -157.00-114.00   0.50    0.80    --  -88.50 -82.00  -6.31   86
 71  \w   -156.00-116.00   0.50    0.80    --  -88.50 -81.00  27.19   80
 72  \w   -160.00-101.00   0.50    0.80    --  -88.50 -83.00 114.21  118
 73  \w   -158.00 -63.00   0.50    0.80    --  -88.50 -81.00 167.17  190
 74  \w   -156.00 -66.00   0.50    0.80    --  -88.50 -77.00 -30.00  180
 75  \w   -145.00 -65.00   0.50    0.80    --  -88.50 -77.00-114.30  160
 76  \w   -160.00-124.00   0.50    0.80    --  -88.50 -77.00-180.00   72
 77  \w   -160.00-103.00   0.50    0.80    --  -88.50 -81.00 -98.25  114
 78  \w   -160.00-131.00   0.50    0.80    --  -88.50 -82.00-159.73   58
 79  \w   -158.00-132.00   0.50    0.80    --  -88.50 -71.00-150.40   52
;
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            95245
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.216
_diffrn_reflns_theta_min         2.942
_exptl_absorpt_coefficient_mu    4.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68073
_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    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 6418 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1008
_refine_ls_number_reflns         14260
_refine_ls_number_restraints     999
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+16.2779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.881
_reflns_number_gt                13898
_reflns_number_total             14260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00031d3.cif
_cod_data_source_block           2d
_cod_depositor_comments
'Adding full bibliography for 7706697--7706707.cif.'
_cod_original_cell_volume        7267.98(10)
_cod_database_code               7706702
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.362
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl5-C71 = Cl3-C70 = Cl4-C70 = Cl6-C71
 1.73 with sigma of 0.01
 Cu1-Cu4 \\sim Cu1-Cu2 \\sim Cu1-Cu3 \\sim Cu4-Cu2 \\sim Cu4-Cu3 \\sim Cu2-Cu3
 with sigma of 0.02
 H-Cu1 \\sim H-Cu4 \\sim H-Cu2 \\sim H-Cu3
 with sigma of 0.01
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(H) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C13A)=Sof(H13A)=Sof(C12A)=Sof(C17A)=Sof(H17A)=Sof(C16A)=Sof(H16A)=
 Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(H14A)=1-FVAR(1)
 Sof(C13)=Sof(H13)=Sof(C12)=Sof(C17)=Sof(H17)=Sof(C16)=Sof(H16)=Sof(C15)=
 Sof(H15)=Sof(C14)=Sof(H14)=FVAR(1)
 Sof(C42A)=Sof(H42A)=Sof(C41A)=Sof(C46A)=Sof(H46A)=Sof(C45A)=Sof(H45A)=
 Sof(C44A)=Sof(H44A)=Sof(C43A)=Sof(H43A)=1-FVAR(2)
 Sof(C42)=Sof(H42)=Sof(C41)=Sof(C46)=Sof(H46)=Sof(C45)=Sof(H45)=Sof(C44)=
 Sof(H44)=Sof(C43)=Sof(H43)=FVAR(2)
 Fixed Sof: Cl5(0.5) Cl4(0.5) Cl6(0.5) Cl3(0.5) N9A(0.6) N10A(0.6) N9(0.4)
 N10(0.4) C71(0.5) H71A(0.5) H71B(0.5) C70(0.5) H70A(0.5) H70B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C71(H71A,H71B), C70(H70A,H70B)
5.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C59(H59), C51(H51), C23(H23), C21(H21), C62(H62), C57(H57), C4(H4),
 C34(H34), C29(H29), C33(H33), C32(H32), C1(H1), C11(H11), C31(H31), C22(H22),
 C50(H50), C61(H61), C65(H65), C66(H66), C60(H60), C67(H67), C68(H68), C28(H28),
  C3(H3), C7(H7), C53(H53), C49(H49), C55(H55), C37(H37), C9(H9), C2(H2),
 C63(H63), C27(H27), C39(H39), C42A(H42A), C46A(H46A), C45A(H45A), C44A(H44A),
 C43A(H43A), C19(H19), C40(H40), C36(H36), C56(H56), C38(H38), C8(H8), C20(H20),
  C54(H54), C26(H26), C10(H10), C25(H25), C13A(H13A), C17A(H17A), C16A(H16A),
 C15A(H15A), C14A(H14A), C13(H13), C17(H17), C16(H16), C15(H15), C14(H14),
 C42(H42), C46(H46), C45(H45), C44(H44), C43(H43)
5.c Fitted hexagon refined as free rotating group:
 C42A(C41A,C46A,C45A,C44A,C43A), C13A(C12A,C17A,C16A,C15A,C14A), C13(C12,C17,
 C16,C15,C14), C42(C41,C46,C45,C44,C43)
;
_shelx_res_checksum              5285
_shelx_hkl_checksum              502
_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
;