Effect of the dangling aromatic ring on neutral luminescent bis(phosphine) Cu(i)/Ag(i) complexes with the asymmetric pyridyl-tetrazolate ligands
Xiang, Jing; Wang, Li-Xin; Zhang, Xu; Zhu, De-Sheng; Wang, Lei; Liu, Lu-Lu; Leung, Chi-Fai; Xiang, Jing; RSC Advances 12 (2022) 27267–27274; doi:10.1039/D2RA04684A

data_7245566
_publ_section_title
;
 Effect of the dangling aromatic ring on neutral luminescent
 bis(phosphine) Cu(i)/Ag(i) complexes with the asymmetric
 pyridyl-tetrazolate ligands
;
_journal_issue                   42
_journal_name_full               'RSC Advances'
_journal_page_first              27267
_journal_page_last               27274
_journal_paper_doi               10.1039/D2RA04684A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         '0.235(C41.5 H32.8 Cu N9 P2)'
_chemical_formula_sum            'C9.76 H7.72 Cu0.24 N2.12 P0.47'
_chemical_formula_weight         184.25
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-26
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2022-06-11 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.9860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            17
_cell_length_a                   18.9696(2)
_cell_length_b                   10.51280(10)
_cell_length_c                   19.2832(2)
_cell_measurement_reflns_used    22721
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.8400
_cell_measurement_theta_min      4.6660
_cell_volume                     3845.53(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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    -82.00 -34.00   0.50    1.00    --    0.00 -38.00-120.00   96
  2  \w    -66.00 -22.00   0.50    1.00    --    0.00 -38.00 -60.00   88
  3  \w    -16.00  87.00   0.50    1.00    --    0.00  38.00-120.00  206
  4  \w     33.00  69.00   0.50    5.20    --   95.20 -45.00   0.00   72
  5  \w     76.00 185.00   0.50    5.20    --   95.20  15.00-150.00  218
  6  \w      8.00 110.00   0.50    5.20    --   95.20 -30.00  30.00  204
  7  \w     23.00 124.00   0.50    5.20    --   95.20 -77.00-150.00  202
  8  \w    -62.00   7.00   0.50    1.00    --    0.00 -38.00   0.00  138
  9  \w    -29.00  -3.00   0.50    1.00    --    0.00 -38.00 120.00   52
 10  \w     46.00  78.00   0.50    1.00    --    0.00  38.00 -30.00   64
 11  \w    -51.00 -11.00   0.50    1.00    --    0.00 -38.00  60.00   80
 12  \w    -71.00 -33.00   0.50    1.00    --    0.00 -38.00 120.00   76
 13  \w     92.00 124.00   0.50    5.20    --   95.20 -82.00  90.00   64
 14  \w      8.00 119.00   0.50    5.20    --   95.20 -61.00 -90.00  222
 15  \w     84.00 113.00   0.50    5.20    --   95.20 -82.00 150.00   58
 16  \w     31.00  57.00   0.50    5.20    --   95.20 -82.00-150.00   52
 17  \w     77.00 103.00   0.50    5.20    --   95.20 -15.00 -90.00   52
 18  \w     81.00 108.00   0.50    5.20    --   95.20 -82.00-150.00   54
 19  \w     12.00  38.00   0.50    5.20    --   95.20 -82.00  60.00   52
 20  \w     52.00 127.00   0.50    5.20    --   95.20 -82.00  60.00  150
 21  \w     90.00 185.00   0.50    5.20    --   95.20  15.00 150.00  190
 22  \w     27.00  53.00   0.50    5.20    --   95.20 -61.00  30.00   52
 23  \w     79.00 176.00   0.50    5.20    --   95.20  30.00-120.00  194
 24  \w     25.00 127.00   0.50    5.20    --   95.20 -82.00 -90.00  204
 25  \w     56.00 118.00   0.50    5.20    --   95.20 -61.00  30.00  124
 26  \w      8.00  71.00   0.50    5.20    --   95.20 -15.00 -90.00  126
 27  \w     46.00  77.00   0.50    5.20    --   95.20 -82.00 150.00   62
 28  \w     93.00 119.00   0.50    5.20    --   95.20 -82.00-180.00   52
 29  \w     79.00 104.00   0.50    5.20    --   95.20 -82.00   0.00   50
 30  \w     85.00 110.00   0.50    5.20    --   95.20 -82.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0707461000
_diffrn_orient_matrix_UB_12      -0.0334243000
_diffrn_orient_matrix_UB_13      0.0346904000
_diffrn_orient_matrix_UB_21      0.0382269000
_diffrn_orient_matrix_UB_22      -0.0937286000
_diffrn_orient_matrix_UB_23      0.0485342000
_diffrn_orient_matrix_UB_31      0.0112712000
_diffrn_orient_matrix_UB_32      0.1075995000
_diffrn_orient_matrix_UB_33      0.0531405000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41771
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.149
_diffrn_reflns_theta_min         3.268
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1615
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.999
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7724
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1290P)^2^+10.5118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6907
_reflns_number_total             7724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra04684a2.cif
_cod_data_source_block           l70+cu
_cod_database_code               7245566
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.831
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Fixed Sof: C40(0.7) C41(0.7) H41(0.7) C42(0.7) H42(0.7) C43(0.7) H43(0.7)
 C44(0.7) H44(0.7)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6A), C5(H5), C15(H15), C27(H27), C25(H25), C13(H13), C14(H14),
 C26(H26), C23(H23), C11(H11), C24(H24), C12(H12), C35(H35), C17(H17), C36(H36),
  C21(H21), C18(H18), C19(H19), C33(H33), C37(H37), C39(H39), C38(H38),
 C29(H29), C20(H20), C31(H31), C32(H32), C30(H30), C41(H41), C42(H42), C43(H43),
  C44(H44), C8(H8)
;
_shelx_res_checksum              63603
_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 5.836
_oxdiff_exptl_absorpt_empirical_full_min 0.436