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_7248623
_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             2024-04-02
_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                97.3254(10)
_cell_angle_beta                 104.5536(10)
_cell_angle_gamma                103.6389(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8439(4)
_cell_length_b                   18.8172(5)
_cell_length_c                   20.8187(6)
_cell_measurement_reflns_used    9511
_cell_measurement_temperature    200.0(1)
_cell_measurement_theta_max      29.852
_cell_measurement_theta_min      2.549
_cell_volume                     4277.4(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0(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'
_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  0.0300
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            386877
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.148
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    5.066
_exptl_absorpt_correction_T_max  0.5644
_exptl_absorpt_correction_T_min  0.4840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0676 before and 0.0490 after correction.
The Ratio of minimum to maximum transmission is 0.8575.
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    2.060
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         19652
_refine_ls_number_restraints     737
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0223P)^2^+10.7421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17398
_reflns_number_total             19652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00173g2.cif
_cod_data_source_block           CP1_200K
_cod_depositor_comments
'Adding full bibliography for 7248612--7248631.cif.'
_cod_database_code               7248623
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C64B-C59B = C64A-C59A = C64B-C63B = C64A-C63A = C63A-C62A = C63B-C62B = C62A-
 C61A = C62B-C61B = C61A-C60A = C61B-C60B = C60A-C59A = C60B-C59B = C54A-C49A =
 C50B-C49B = C54A-C53A = C51B-C50B = C53A-C52A = C52B-C51B = C52A-C51A = C53B-
 C52B = C51A-C50A = C54B-C53B = C50A-C49A = C54B-C49B = C32B-C27 = C32A-C27 =
 C32B-C31B = C31B-C30B = C30B-C29B = C29B-C28B = C28B-C27 = C32A-C31A = C31A-
 C30A = C30A-C29A = C29A-C28A = C28A-C27 = C22A-C17A = C22B-C17B = C22B-C21B =
 C21B-C20B = C21A-C20A = C20B-C19B = C20A-C19A = C18B-C17B = C19A-C18A = C18A-
 C17A = C19B-C18B = C6B-C1B = C6A-C1A = C6A-C5A = C6B-C5B = C5A-C4A = C5B-C4B =
 C4B-C3B = C4A-C3A = C3B-C2B = C3A-C2A = C2A-C1A = C2B-C1B
 1.5 with sigma of 0.05
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=
 Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6BA)=
 Sof(H6BB)=1-FVAR(1)
 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)=FVAR(1)
 Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18C)=Sof(H18D)=Sof(C19B)=Sof(H19C)=
 Sof(H19D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=Sof(H21C)=Sof(H21D)=
 Sof(C22B)=Sof(H22C)=Sof(H22D)=1-FVAR(2)
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(C19A)=Sof(H19A)=
 Sof(H19B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(H21A)=Sof(H21B)=
 Sof(C22A)=Sof(H22A)=Sof(H22B)=FVAR(2)
 Sof(H27A)=Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29C)=Sof(H29D)=
 Sof(C30B)=Sof(H30C)=Sof(H30D)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=
 Sof(H32C)=Sof(H32D)=1-FVAR(3)
 Sof(H27)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=
 Sof(H32A)=Sof(H32B)=FVAR(3)
 Sof(C49B)=Sof(H49B)=Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=Sof(H51C)=
 Sof(H51D)=Sof(C52B)=Sof(H52C)=Sof(H52D)=Sof(C53B)=Sof(H53C)=Sof(H53D)=
 Sof(C54B)=Sof(H54C)=Sof(H54D)=1-FVAR(4)
 Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(C51A)=Sof(H51A)=
 Sof(H51B)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(C53A)=Sof(H53A)=Sof(H53B)=
 Sof(C54A)=Sof(H54A)=Sof(H54B)=FVAR(4)
 Sof(C59B)=Sof(H59B)=Sof(C60B)=Sof(H60C)=Sof(H60D)=Sof(C61B)=Sof(H61C)=
 Sof(H61D)=Sof(C62B)=Sof(H62C)=Sof(H62D)=Sof(C63B)=Sof(H63C)=Sof(H63D)=
 Sof(C64B)=Sof(H64C)=Sof(H64D)=1-FVAR(5)
 Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(C61A)=Sof(H61A)=
 Sof(H61B)=Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(C63A)=Sof(H63A)=Sof(H63B)=
 Sof(C64A)=Sof(H64A)=Sof(H64B)=FVAR(5)
5.a Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B), C11(H11), C17A(H17A), C17B(H17B), C27(H27), C27(H27A),
 C33(H33), C43(H43), C49A(H49A), C49B(H49B), C59A(H59A), C59B(H59B)
5.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4A(H4AA,
 H4AB), C4B(H4BA,H4BB), C5A(H5AA,H5AB), C5B(H5BA,H5BB), C6A(H6AA,H6AB),
 C6B(H6BA,H6BB), C7(H7A,H7B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18A(H18A,H18B), C18B(H18C,
 H18D), C19A(H19A,H19B), C19B(H19C,H19D), C20A(H20A,H20B), C20B(H20C,H20D),
 C21A(H21A,H21B), C21B(H21C,H21D), C22A(H22A,H22B), C22B(H22C,H22D), C23(H23A,
 H23B), C26(H26A,H26B), C28A(H28A,H28B), C28B(H28C,H28D), C29A(H29A,H29B),
 C29B(H29C,H29D), C30A(H30A,H30B), C30B(H30C,H30D), C31A(H31A,H31B), C31B(H31C,
 H31D), C32A(H32A,H32B), C32B(H32C,H32D), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C42(H42A,H42B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C50A(H50A,H50B), C50B(H50C,H50D), C51A(H51A,H51B), C51B(H51C,H51D),
 C52A(H52A,H52B), C52B(H52C,H52D), C53A(H53A,H53B), C53B(H53C,H53D), C54A(H54A,
 H54B), C54B(H54C,H54D), C55(H55A,H55B), C58(H58A,H58B), C60A(H60A,H60B),
 C60B(H60C,H60D), C61A(H61A,H61B), C61B(H61C,H61D), C62A(H62A,H62B), C62B(H62C,
 H62D), C63A(H63A,H63B), C63B(H63C,H63D), C64A(H64A,H64B), C64B(H64C,H64D)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.476
_shelx_estimated_absorpt_t_max   0.676
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              44641