Polymeric CuX coordination compounds assembled from acetylenic thioether ligands RSCH2CCCH2R (R = C6H11, t-Bu): effect of the RS-group, halide and stoichiometry on the network architecture and the luminescence properties
Knorr, Michael; Viau, Lydie; Knauer, Lena; Strohmann, Carsten; Rousselin, Yoann; Kubicki, Marek M.; CrystEngComm 26 (2024) 2953–2975; doi:10.1039/D4CE00173G

data_7248621
_publ_section_title
;
 Polymeric CuX coordination compounds assembled from acetylenic thioether
 ligands RSCH2C&#xE002;CCH2R (R = C6H11, t-Bu): effect of the RS-group,
 halide and stoichiometry on the network architecture and the luminescence
 properties
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              2953
_journal_page_last               2975
_journal_paper_doi               10.1039/D4CE00173G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C64 H104 Cu8 I8 S8'
_chemical_formula_sum            'C64 H104 Cu8 I8 S8'
_chemical_formula_weight         2653.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-04-03
_audit_creation_method
;FinalCif V136 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-04-08 deposited with the CCDC.	2024-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                96.658(4)
_cell_angle_beta                 105.219(4)
_cell_angle_gamma                105.342(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9606(16)
_cell_length_b                   19.095(3)
_cell_length_c                   21.026(3)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    300.0(1)
_cell_measurement_theta_max      32.82
_cell_measurement_theta_min      2.28
_cell_volume                     4379.0(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      300.0(1)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CPAD PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a~1~'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            100554
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.024
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    4.948
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0961 before and 0.0585 after correction. The Ratio of minimum to maximum transmission is 0.8754. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.084
_refine_diff_density_max         2.057
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         15416
_refine_ls_number_restraints     675
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0823P)^2^+11.6776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10833
_reflns_number_total             15416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00173g2.cif
_cod_data_source_block           CP1_300K
_cod_depositor_comments
'Adding full bibliography for 7248612--7248631.cif.'
_cod_original_cell_volume        4378.9(10)
_cod_database_code               7248621
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C6-C1 = C2A-C1A = C2-C1 = C6A-C1A = C6A-C5A = C5A-C4A = C5-C4 = C6-C5 = C3A-
 C2A = C4A-C3A = C3-C2 = C4-C3 = C16-C15 = C16-C11 = C16A-C11 = C12-C11 = C12A-
 C11 = C13A-C12A = C15A-C14A = C14-C13 = C15-C14 = C14A-C13A = C16A-C15A = C13-
 C12 = C34A-C33 = C34-C33 = C38A-C33 = C38A-C37A = C37A-C36A = C36-C35 = C35-
 C34 = C35A-C34A = C38-C37 = C37-C36 = C36A-C35A = C38-C33 = C48-C43 = C44A-
 C43A = C48A-C43A = C44-C43 = C45-C44 = C48A-C47A = C46-C45 = C47A-C46A = C47-
 C46 = C46A-C45A = C45A-C44A = C48-C47 = C18-C17 = C22-C17 = C22-C21 = C21-C20 =
  C20-C19 = C19-C18 = C32-C27 = C28-C27 = C29-C28 = C31-C30 = C30-C29 = C32-C31
 = C50-C49 = C54-C49 = C54-C53 = C53-C52 = C52-C51 = C51-C50 = C61-C60 = C64A-
 C63A = C60-C59 = C64A-C59A = C60A-C59A = C64-C59 = C64-C63 = C61A-C60A = C62-
 C61 = C62A-C61A = C63-C62
 1.5 with sigma of 0.005
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45C)=
 Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=Sof(H47C)=Sof(H47D)=
 Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(1)
 Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=
 Sof(H48B)=FVAR(1)
 Sof(H33A)=Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=
 Sof(H38C)=Sof(H38D)=1-FVAR(2)
 Sof(H33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=
 Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 FVAR(2)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=1-FVAR(3)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(3)
 Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(H60C)=Sof(H60D)=Sof(C61A)=Sof(H61C)=
 Sof(H61D)=Sof(C62A)=Sof(H62C)=Sof(H62D)=Sof(C63A)=Sof(H63C)=Sof(H63D)=
 Sof(C64A)=Sof(H64C)=Sof(H64D)=1-FVAR(4)
 Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C61)=Sof(H61A)=Sof(H61B)=
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=
 Sof(H64B)=FVAR(4)
 Sof(H11A)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=
 Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=
 Sof(H16C)=Sof(H16D)=1-FVAR(5)
 Sof(H11)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=
 Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 FVAR(5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A), C11(H11), C11(H11A), C17(H17), C27(H27), C33(H33),
 C33(H33A), C43(H43), C43A(H43A), C49(H49), C59(H59), C59A(H59A)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB), C3(H3A,H3B), C3A(H3AA,H3AB), C4(H4A,H4B),
 C4A(H4AA,H4AB), C5(H5A,H5B), C5A(H5AA,H5AB), C6(H6A,H6B), C6A(H6AA,H6AB),
 C7(H7A,H7B), C10(H10A,H10B), C12(H12A,H12B), C12A(H12C,H12D), C13(H13A,H13B),
 C13A(H13C,H13D), C14(H14A,H14B), C14A(H14C,H14D), C15(H15A,H15B), C15A(H15C,
 H15D), C16(H16A,H16B), C16A(H16C,H16D), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B),
  C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C34(H34A,H34B), C34A(H34C,H34D), C35(H35A,H35B), C35A(H35C,H35D),
 C36(H36A,H36B), C36A(H36C,H36D), C37(H37A,H37B), C37A(H37C,H37D), C38(H38A,
 H38B), C38A(H38C,H38D), C39(H39A,H39B), C42(H42A,H42B), C44(H44A,H44B),
 C44A(H44C,H44D), C45(H45A,H45B), C45A(H45C,H45D), C46(H46A,H46B), C46A(H46C,
 H46D), C47(H47A,H47B), C47A(H47C,H47D), C48(H48A,H48B), C48A(H48C,H48D),
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B),
  C55(H55A,H55B), C58(H58A,H58B), C60(H60A,H60B), C60A(H60C,H60D), C61(H61A,
 H61B), C61A(H61C,H61D), C62(H62A,H62B), C62A(H62C,H62D), C63(H63A,H63B),
 C63A(H63C,H63D), C64(H64A,H64B), C64A(H64C,H64D)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.490
_shelx_estimated_absorpt_t_max   0.681
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              37611