Zero-dimensional Cu(I)-based organometallic halide with green cluster-centred emission for high resolution X-ray imaging screens.
Almushaikeh, Alaa M.; Wang, Hong; Gutiérrez-Arzaluz, Luis; Yin, Jun; Huang, Ren-Wu; Bakr, Osman M.; Mohammed, Omar F.; Chemical communications (Cambridge, England) 59 (2023) 4447–4450; doi:10.1039/d3cc00730h

data_7131605
_publ_section_title
;
 Zero-dimensional Cu(I)-based organometallic halide with green
 cluster-centred emission for high resolution X-ray imaging screens.
;
_journal_issue                   30
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4447
_journal_page_last               4450
_journal_paper_doi               10.1039/d3cc00730h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'Cu4 I6, C24 H48 O12 Rb2, 0.5(C6 H12 O2)'
_chemical_formula_sum            'C27 H54 Cu4 I6 O13 Rb2'
_chemical_formula_weight         1773.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-01-25 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.888(15)
_cell_length_b                   15.243(8)
_cell_length_c                   10.929(6)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      28.509
_cell_measurement_theta_min      2.288
_cell_volume                     5146(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      260.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            48321
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.471
_diffrn_reflns_theta_min         2.283
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    7.157
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0688 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.8023.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_description       block
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         8044
_refine_ls_number_restraints     638
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0118P)^2^+24.0806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5656
_reflns_number_total             8044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00730h2.cif
_cod_data_source_block           20221102a_rbcui_0m
_cod_database_code               7131605
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.456
_shelx_estimated_absorpt_t_min   0.268
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C24 \\sim C14-C23 \\sim C26-C11 \\sim C13-C7 \\sim C12-C6 \\sim C15-C4
 with sigma of 0.01
 O2-C25 \\sim O2-C23 \\sim O5-C24 \\sim O5-C4 \\sim O8-C15 \\sim O8-C6 \\sim
O10-C12 \\sim O10-C7 \\sim O4-C13
 \\sim O4-C26 \\sim O6-C11 \\sim O6-C14
 with sigma of 0.01
 C2-C1 \\sim C27-C1
 with sigma of 0.01
 C2-O13 \\sim O13-C27
 with sigma of 0.01
 O3-C9 \\sim O3-C5 \\sim O7-C18 \\sim O7-C10 \\sim O12-C20 \\sim O12-C8 \\sim
O9-C16 \\sim O9-C19 \\sim O1-C17
 \\sim O1-C3 \\sim O11-C21 \\sim O11-C22
 with sigma of 0.01
 C9-C22 \\sim C21-C3 \\sim C17-C19 \\sim C8-C16 \\sim C10-C20 \\sim C18-C5
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O2 \\sim O4 \\sim O5 \\sim O6 \\sim O8 \\sim O10 \\sim C4 \\sim C6 \\sim C7
\\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C23 \\sim C24 \\sim C25
\\sim C26: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O13 \\sim C1 \\sim C2 \\sim C27: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1 \\sim O3 \\sim O7 \\sim O9 \\sim O11 \\sim O12 \\sim C3 \\sim C5 \\sim C8
\\sim C9 \\sim C10 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21
\\sim C22: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C27 \\sim O13 \\sim C1 \\sim C2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O13)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O2, O4, O5, O6, O8, O10, C4, C6, C7, C11, C12, C13, C14, C15, C23, C24, C25,
 C26
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O1, O3, O7, O9, O11, O12, C3, C5, C8, C9, C10, C16, C17, C18, C19, C20, C21,
 C22
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Fixed Sof: Cu3(0.4375) Cu4(0.875) Cu5(0.4375) Cu6(0.125) Cu7(0.0625)
 Cu8(0.0625) O2(0.5) O4(0.5) O5(0.5) O6(0.5) O8(0.5) O10(0.5) C4(0.5) H4A(0.5)
 H4B(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C11(0.5)
 H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5) C13(0.5) H13A(0.5) H13B(0.5)
 C14(0.5) H14A(0.5) H14B(0.5) C15(0.5) H15A(0.5) H15B(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) C24(0.5) H24A(0.5) H24B(0.5) C25(0.5) H25A(0.5) H25B(0.5) C26(0.5)
 H26A(0.5) H26B(0.5) O1(0.5) O3(0.5) O7(0.5) O9(0.5) O11(0.5) O12(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5)
 H9A(0.5) H9B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 C17(0.5) H17A(0.5) H17B(0.5) C18(0.5) H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5) C21(0.5) H21A(0.5) H21B(0.5) C22(0.5)
 H22A(0.5) H22B(0.5) O13(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C27(0.5)
 H27A(0.5) H27B(0.5) H27C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C23(H23A,H23B), C24(H24A,H24B),
  C25(H25A,H25B), C26(H26A,H26B), C3(H3A,H3B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,
 H9B), C10(H10A,H10B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C27(H27A,H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'