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_7706697
_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
'1.5(C68 H60 Cu5.333 N4 P4), C2 H4 Cl4, F12 P2'
_chemical_formula_sum            'C104 H94 Cl4 Cu8 F12 N6 P8'
_chemical_formula_weight         2553.73
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   25.4756(5)
_cell_length_b                   25.4756(5)
_cell_length_c                   13.9849(4)
_cell_measurement_reflns_used    5027
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.4200
_cell_measurement_theta_min      3.4560
_cell_volume                     7860.3(3)
_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_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0734
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22580
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        66.739
_diffrn_reflns_theta_max         66.739
_diffrn_reflns_theta_min         3.160
_exptl_absorpt_coefficient_mu    4.434
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49439
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         8942
_refine_ls_number_restraints     834
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0769
_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^)+(0.1400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2073
_refine_ls_wR_factor_ref         0.2367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5206
_reflns_number_total             8942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00031d3.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7706697--7706707.cif.
;
_cod_original_cell_volume        7860.3(4)
_cod_database_code               7706697
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 HF-Cu6 \\sim HF-Cu6_$3 \\sim HF-Cu6_$4
 with sigma of 0.02
 H-Cu2 \\sim H-Cu3 \\sim H-Cu3_$2
 with sigma of 0.02
 HC-Cu2 \\sim HC-Cu2_$1 \\sim HC-Cu3
 with sigma of 0.02
 HA-Cu1 \\sim HA-Cu2 \\sim HA-Cu2_$1 \\sim HA-Cu2_$2
 with sigma of 0.02
 HD-Cu4 \\sim HD-Cu3 \\sim HD-Cu3_$1 \\sim HD-Cu3_$2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(HD) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Same fragment restrains
{C12, C13, C14, C15, C16, C17} sigma for 1-2: 0.02, 1-3: 0.04
as
{C12', C13', C14', C15', C16', C17'}
{P4, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.02, 1-3: 0.04
as
{P4', F1', F2', F3', F4', F5', F6'}
5. Others
 Sof(C12')=Sof(C13')=Sof(H13')=Sof(C14')=Sof(H14')=Sof(C15')=Sof(H15')=
 Sof(C16')=Sof(H16')=Sof(C17')=Sof(H17')=1-FVAR(1)
 Sof(C12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=
 Sof(H16)=Sof(C17)=Sof(H17)=FVAR(1)
 Sof(P4')=Sof(F1')=Sof(F2')=Sof(F3')=Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(2)
 Sof(P4)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Fixed Sof: HA(0.03333) HB(0.3) H(0.66667) HC(0.66667) HF(0.66667)
 Fixed Uiso: HA(0.06) HB(0.06) H(0.06) HC(0.06) HE(0.06) HF(0.06)
6.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C13'(H13'), C14'(H14'),
 C15'(H15'), C16'(H16'), C17'(H17'), C19(H19), C20(H20), C21(H21), C22(H22),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51)
;
_shelx_res_checksum              27167
_shelx_hkl_checksum              65769
_olex2_submission_special_instructions 'No special instructions were received'