Convenient synthesis of copper(I) halide quasi-one-dimensional coordination polymers: their structures and solid-state luminescent properties.
Masahara, Shingo; Yokoyama, Hiromichi; Suzaki, Yuji; Ide, Tomohito; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8889–8898; doi:10.1039/d1dt01571k

data_7707455
_publ_section_title
;
 Convenient synthesis of copper(I) halide quasi-one-dimensional
 coordination polymers: their structures and solid-state luminescent
 properties.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8889
_journal_page_last               8898
_journal_paper_doi               10.1039/d1dt01571k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '3(C21 H27 Cl1 Cu1 N3)'
_chemical_formula_sum            'C63 H81 Cl3 Cu3 N9'
_chemical_formula_weight         1261.33
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-13 deposited with the CCDC.	2021-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   14.7196(5)
_cell_length_b                   14.7196(5)
_cell_length_c                   8.3670(4)
_cell_measurement_reflns_used    1527
_cell_measurement_temperature    90
_cell_measurement_theta_max      76.2530
_cell_measurement_theta_min      8.7270
_cell_volume                     1569.97(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.955
_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    -14.00  55.00   0.50    0.05    --   46.45-100.00  21.00  138
  2  \w     34.00  70.00   0.50    0.05    --  104.61 -61.00 -30.00   72
  3  \w     35.00  61.00   0.50    0.05    --  104.61 -61.00 -60.00   52
  4  \w     92.00 117.00   0.50    0.05    --  104.61  24.00 -22.00   50
  5  \w    140.00 178.00   0.50    0.05    --  104.61  24.00 -22.00   76
  6  \w     -3.00  29.00   0.50    0.05    --  -46.45  19.00 120.00   64
  7  \w    -64.00 -33.00   0.50    0.05    -- -102.00  61.00 120.00   62
  8  \w    -69.00 -44.00   0.50    0.05    -- -102.00  61.00  60.00   50
  9  \w    -68.00 -42.00   0.50    0.05    -- -102.00  61.00 -60.00   52
 10  \w    -63.00 -38.00   0.50    0.05    -- -102.00  58.00-105.00   50
 11  \w   -169.00 -90.00   0.50    0.05    -- -102.00 -34.00 127.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1053457000
_diffrn_orient_matrix_UB_12      0.0094583000
_diffrn_orient_matrix_UB_13      -0.0486249000
_diffrn_orient_matrix_UB_21      -0.0104233000
_diffrn_orient_matrix_UB_22      0.0364408000
_diffrn_orient_matrix_UB_23      -0.1681094000
_diffrn_orient_matrix_UB_31      0.0583871000
_diffrn_orient_matrix_UB_32      0.1148640000
_diffrn_orient_matrix_UB_33      0.0573544000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0119
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1562
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.408
_diffrn_reflns_theta_min         8.746
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.701
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       needle
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.314
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         679
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0170
_refine_ls_R_factor_gt           0.0170
_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^)+(0.0221P)^2^+1.5759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0456
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.734
_reflns_Friedel_fraction_max     0.676
_reflns_number_gt                679
_reflns_number_total             679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01571k2.cif
_cod_data_source_block           hy327
_cod_depositor_comments
'Adding full bibliography for 7707451--7707455.cif.'
_cod_original_cell_volume        1569.97(13)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               7707455
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.484
_shelx_estimated_absorpt_t_min   0.355
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(3)
 0.11(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C1(H1), C3(H3)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              49754
_shelx_hkl_checksum              98367
_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 1.201
_oxdiff_exptl_absorpt_empirical_full_min 0.873