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_7706707
_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         'C51 H43 Cu4 I3 N3 P3, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C52.5 H46 Cl3 Cu4 I3 N3 P3'
_chemical_formula_weight         1553.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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            16
_cell_length_a                   49.0830(4)
_cell_length_b                   37.3456(3)
_cell_length_c                   11.73950(10)
_cell_measurement_reflns_used    21489
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.7940
_cell_measurement_theta_min      2.9750
_cell_volume                     21518.9(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.966
_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    -62.00 -33.00   0.50    2.00    --  -46.75  37.00-150.00   58
  2  \w    -27.00  27.00   0.50    2.00    --  -46.75  37.00-150.00  108
  3  \w    -76.00 -29.00   0.50    8.00    --  -88.50 100.00 -37.00   94
  4  \w    -88.00 -13.00   0.50    2.00    --  -46.75 123.00  41.00  150
  5  \w   -104.00 -79.00   0.50    2.00    --  -46.75-125.00   0.00   50
  6  \w   -160.00-106.00   0.50    8.00    --  -88.50 -45.00-150.00  108
  7  \w     35.00 121.00   0.50    8.00    --  107.31 -25.00  25.00  172
  8  \w     67.00  99.00   0.50    8.00    --  107.31 -94.00   0.00   64
  9  \w     80.00 107.00   0.50    8.00    --  107.31 -94.00  90.00   54
 10  \w     39.00  65.00   0.50    8.00    --  107.31 -94.00  90.00   52
 11  \w     33.00 116.00   0.50    8.00    --  107.31 -30.00 -60.00  166
 12  \w     38.00 103.00   0.50    8.00    --  107.31 -45.00 -90.00  130
 13  \w    103.00 178.00   0.50    8.00    --  107.31 123.00  41.00  150
;
_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  0.0294
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25258
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.008
_diffrn_reflns_theta_min         2.974
_exptl_absorpt_coefficient_mu    17.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68548
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_description       block
_exptl_crystal_F_000             12048
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 3651 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0095(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         9639
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+56.4818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.672
_reflns_Friedel_fraction_full    0.793
_reflns_Friedel_fraction_max     0.717
_reflns_number_gt                9410
_reflns_number_total             9639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00031d3.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 7706697--7706707.cif.'
_cod_original_formula_sum        'C52.50 H46 Cl3 Cu4 I3 N3 P3'
_cod_database_code               7706707
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.470
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(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
 Fixed Sof: H51A(0.5) H51B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C51(H51A,H51B)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C12(H12), C4(H4), C20(H20), C6(H6), C17(H17), C21(H21), C41(H41),
 C30(H30), C25(H25), C50(H50), C5(H5), C44(H44), C47(H47), C43(H43), C16(H16),
 C26(H26), C33(H33), C28(H28), C11(H11), C14(H14), C39(H39), C48(H48), C23(H23),
  C27(H27), C10(H10), C49(H49), C22(H22), C3(H3), C19(H19), C42(H42), C9(H9),
 C01K(H01K), C8(H8), C31(H31), C32(H32), C2(H2), C36(H36), C35(H35), C37(H37),
 C45(H45), C38(H38)
;
_shelx_res_checksum              36593
_shelx_hkl_checksum              90356
_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
;