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_7713505
_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 Br Cu N, C2 H3 N'
_chemical_formula_sum            'C22.5 H21 As Br Cu N2'
_chemical_formula_weight         537.78
_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                 93.153(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0669(3)
_cell_length_b                   17.9010(7)
_cell_length_c                   13.4554(6)
_cell_measurement_reflns_used    3172
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      25.3080
_cell_measurement_theta_min      2.8470
_cell_volume                     2180.59(15)
_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      93.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -74.00 -42.00   0.10    6.50    --   30.00  54.00-120.00  320
  2  \w    -26.00  12.00   0.10    6.50    --   30.00  54.00-120.00  380
  3  \w    -63.00 119.00   0.10    6.50    --   30.00  54.00-180.00 1820
;
_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      -0.0527718000
_diffrn_orient_matrix_UB_12      -0.0208307000
_diffrn_orient_matrix_UB_13      0.0254375000
_diffrn_orient_matrix_UB_21      0.0468880000
_diffrn_orient_matrix_UB_22      -0.0316961000
_diffrn_orient_matrix_UB_23      -0.0000948000
_diffrn_orient_matrix_UB_31      0.0340470000
_diffrn_orient_matrix_UB_32      0.0114520000
_diffrn_orient_matrix_UB_33      0.0462486000
_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  0.0242
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8978
_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         25.349
_diffrn_reflns_theta_min         2.521
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80987
_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    1.638
_exptl_crystal_description       plate
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3977
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0251P)^2^+3.7101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3205
_reflns_number_total             3977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00784g2.cif
_cod_data_source_block           '[Cu2Br2(AsPh3)2(meprz)]n_93K'
_cod_original_formula_sum        'C22.50 H21 As Br Cu N2'
_cod_database_code               7713505
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHAsCuBrN
_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
 N2A-C22A \\sim N2B-C22B
 with sigma of 0.02
 C22A-C23A \\sim C22B-C23B
 with sigma of 0.02
 N2A-C23A \\sim N2B-C23B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C23A \\sim C22A \\sim N2B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N2A \\sim C22B \\sim C23B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C23B, C22B, N2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2A, C22A, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2A, C22B, C23B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C19, C20, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C22B)=Sof(N2B)=1-FVAR(1)
 Sof(N2A)=Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Fixed Sof: H19(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C14(H14), C6(H6), C18(H18), C8(H8), C2(H2), C4(H4),
 C9(H9), C17(H17), C16(H16), C5(H5), C15(H15), C3(H3), C10(H10), C12(H12),
 C11(H11)
6.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23A(H23A,H23B,H23C), C23B(H23D,H23E,H23F)
;
_shelx_res_checksum              27818
_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.843