Robust and highly emissive copper(I) halide 1D-coordination polymers with triphenylarsine and a series of bridging N-heteroaromatic co-ligands
Kikuchi, Kazuma; Imoto, Hiroaki; Naka, Kensuke; Dalton Transactions  (2023) –; doi:10.1039/D3DT00784G

data_7713508
_publ_section_title
;
 Robust and highly emissive copper(I) halide 1D-coordination polymers with
 triphenylarsine and a series of bridging N-heteroaromatic co-ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00784G
_journal_year                    2023
_chemical_formula_moiety         'C20.5 H18 As Cu I N, C2 H4 N'
_chemical_formula_sum            'C22.5 H22 As Cu I N2'
_chemical_formula_weight         585.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-26
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-05-31 deposited with the CCDC.	2023-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.323(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9916(5)
_cell_length_b                   18.7540(8)
_cell_length_c                   13.3544(7)
_cell_measurement_reflns_used    2406
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1910
_cell_measurement_theta_min      3.0710
_cell_volume                     2245.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -35.00  10.00   0.20    2.00    --   30.00  54.00  30.00  225
  2  \w    -65.00 119.00   0.20    2.00    --   30.00  54.00 -60.00  920
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0150507000
_diffrn_orient_matrix_UB_12      -0.0361727000
_diffrn_orient_matrix_UB_13      0.0123506000
_diffrn_orient_matrix_UB_21      -0.0770262000
_diffrn_orient_matrix_UB_22      -0.0080452000
_diffrn_orient_matrix_UB_23      -0.0078544000
_diffrn_orient_matrix_UB_31      0.0093560000
_diffrn_orient_matrix_UB_32      -0.0075118000
_diffrn_orient_matrix_UB_33      -0.0512756000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8400
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         2.518
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
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    1.733
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.532
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.269
_refine_diff_density_max         1.488
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4097
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0528P)^2^+7.4592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3003
_reflns_number_total             4097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00784g2.cif
_cod_data_source_block           '[Cu2I2(AsPh3)2(meprz)]n_298K'
_cod_original_formula_sum        'C22.50 H22 As Cu I N2'
_cod_database_code               7713508
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHAsCuIN
_shelx_estimated_absorpt_t_max   0.426
_shelx_estimated_absorpt_t_min   0.236
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2B-C22B \\sim N2A-C22A
 with sigma of 0.02
 C22B-C23B \\sim C22A-C23A
 with sigma of 0.02
 N2B-C23B \\sim N2A-C23A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N2A \\sim C22B \\sim C23A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N2B \\sim C22A \\sim C23B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C14, C13, C18, C17, C16, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C12, C11, C10, C9, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C5, C4, C3, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23B, C22A, N2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22B, C23A, N2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C19, N1, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H19(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) N2B(0.5) C22B(0.5)
 H22B(0.5) C23B(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C23A(0.5) H23D(0.5)
 H23E(0.5) H23F(0.5) C22A(0.5) H22A(0.5) N2A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C10(H10), C9(H9), C8(H8), C19(H19), C20(H20), C18(H18),
 C17(H17), C16(H16), C15(H15), C14(H14), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2),
  C22B(H22B), C22A(H22A)
6.b Fitted hexagon refined as free rotating group:
 C7(C12,C11,C10,C9,C8), C18(C17,C16,C15,C14,C13), C6(C5,C4,C3,C2,C1)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23B(H23A,H23B,H23C), C23A(H23D,H23E,H23F)
;
_shelx_res_checksum              85846
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.565
_oxdiff_exptl_absorpt_empirical_full_min 0.801