Ethynyl π-coordinated and non-coordinated mononuclear Cu(i) halide diphosphine complexes: synthesis and photophysical studies
Liu, Nian; Liu, Li; Zhong, Xin-Xin; Li, Fa-Bao; Li, Feng-Yan; Qin, Hai-Mei; New Journal of Chemistry 46 (2022) 3236–3247; doi:10.1039/D1NJ05578J

data_7061200
_publ_section_title
;
 Ethynyl \p-coordinated and non-coordinated mononuclear Cu(i) halide
 diphosphine complexes: synthesis and photophysical studies
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3236
_journal_page_last               3247
_journal_paper_doi               10.1039/D1NJ05578J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C38 H28 Br Cu P2'
_chemical_formula_sum            'C38 H28 Br Cu P2'
_chemical_formula_weight         689.99
_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     dual
_audit_creation_date             2020-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-21 deposited with the CCDC.	2022-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                94.9990(10)
_cell_angle_beta                 101.4460(10)
_cell_angle_gamma                92.0070(10)
_cell_formula_units_Z            2
_cell_length_a                   9.44410(10)
_cell_length_b                   10.0937(2)
_cell_length_c                   16.8020(3)
_cell_measurement_reflns_used    21423
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.6590
_cell_measurement_theta_min      2.6870
_cell_volume                     1561.59(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_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  66.00   0.50    0.10    --   37.97 -50.00   3.00  202
  2  \w     -7.00  19.00   0.50    0.10    --  -37.97  50.00 150.00   52
  3  \w     15.00  42.00   0.50    0.05    --    0.00  50.00 150.00   54
  4  \w     80.00 111.00   0.50    0.10    --   37.97  50.00 150.00   62
  5  \w     41.00  67.00   0.50    0.10    --   37.97  50.00 150.00   52
  6  \w     33.00 146.00   0.50    1.00    --  112.45 -50.00   3.00  226
  7  \w     83.00 178.00   0.50    1.00    --  112.45  50.00 150.00  190
  8  \w     62.00 125.00   0.50    0.10    --   37.97 178.00   0.00  126
  9  \w     61.00 116.00   0.50    0.10    --   37.97 178.00 -60.00  110
 10  \w     63.00 125.00   0.50    0.10    --   37.97 178.00-180.00  124
 11  \w    113.00 149.00   0.50    1.00    --  112.45 178.00-120.00   72
 12  \w     81.00 107.00   0.50    1.00    --  112.45 178.00-120.00   52
 13  \w     60.00 140.00   0.50    1.00    --  112.45 178.00  30.00  160
 14  \w     60.00 120.00   0.50    0.10    --   37.97 178.00 120.00  120
 15  \w     10.00 113.00   0.50    0.10    --   37.97  57.00 -30.00  206
 16  \w     31.00 104.00   0.50    1.00    --  112.45 -94.00   0.00  146
 17  \w     57.00 113.00   0.50    1.00    --  112.45-111.00-120.00  112
 18  \w     65.00 108.00   0.50    1.00    --  112.45 -94.00-180.00   86
 19  \w     31.00 112.00   0.50    1.00    --  112.45-111.00   0.00  162
 20  \w     59.00 107.00   0.50    1.00    --  112.45-111.00 120.00   96
 21  \w    -34.00  -8.00   0.50    0.05    --    0.00  50.00 150.00   52
 22  \w     -6.00  34.00   0.50    0.10    --   37.97  95.00  39.55   80
 23  \w     -5.00  44.00   0.50    0.10    --   37.97  91.00 -51.28   98
 24  \w     -6.00  44.00   0.50    0.10    --   37.97  91.00-132.38  100
 25  \w    -50.00 -12.00   0.50    0.10    --  -37.97 -50.00   3.00   76
 26  \w    -26.00   0.00   0.50    0.10    --  -37.97 -77.00 -60.00   52
 27  \w    -48.00 -23.00   0.50    0.05    --    0.00 -50.00   3.00   50
 28  \w    -33.00  -8.00   0.50    0.10    --  -37.97 -57.00  90.00   50
 29  \w    -59.00 -33.00   0.50    0.10    --  -37.97 -57.00  60.00   52
 30  \w    -71.00 -46.00   0.50    0.10    --  -37.97 -77.00 -60.00   50
 31  \w   -116.00 -74.00   0.50    0.10    --  -37.97 -77.00-180.00   84
 32  \w    -67.00  -1.00   0.50    0.10    --  -37.97 -77.00-180.00  132
 33  \w    -95.00 -59.00   0.50    1.00    --  -98.50 -80.00 -38.84   72
 34  \w    -85.00 -60.00   0.50    1.00    --  -98.50 -78.00  -0.99   50
 35  \w    -88.00 -59.00   0.50    1.00    --  -98.50 -80.00  43.82   58
 36  \w    -83.00 -58.00   0.50    1.00    --  -98.50 -82.00  88.20   50
 37  \w    -97.00 -60.00   0.50    1.00    --  -98.50 -78.00  54.19   74
 38  \w   -101.00 -58.00   0.50    1.00    --  -98.50 -83.00 -12.89   86
 39  \w    -90.00 -58.00   0.50    1.00    --  -98.50 -83.00 -24.55   64
 40  \w    -97.00 -60.00   0.50    1.00    --  -98.50 -77.00-103.70   74
 41  \w    -91.00 -60.00   0.50    1.00    --  -98.50 -80.00-162.75   62
 42  \w    -94.00 -60.00   0.50    1.00    --  -98.50 -77.00-120.00   68
 43  \w   -105.00 -61.00   0.50    1.00    --  -98.50 -74.00 -74.57   88
 44  \w   -105.00 -59.00   0.50    1.00    --  -98.50 -79.00  27.39   92
 45  \w    -90.00 -60.00   0.50    1.00    --  -98.50 -77.00 139.45   60
 46  \w    -96.00 -58.00   0.50    1.00    --  -98.50 -81.00 119.40   76
 47  \w   -106.00 -67.00   0.50    1.00    --  -98.50 -66.00 148.59   78
 48  \w   -116.00 -61.00   0.50    1.00    --  -98.50 -75.00 102.62  110
 49  \w   -116.00 -55.00   0.50    0.10    --  -37.97 -50.00   3.00  122
 50  \w   -100.00 -75.00   0.50    1.00    --  -98.50  50.00 150.00   50
 51  \w   -131.00 -97.00   0.50    1.00    --  -98.50 -50.00   3.00   68
 52  \w   -127.00-102.00   0.50    1.00    --  -98.50 -78.00  -0.99   50
 53  \w   -139.00-103.00   0.50    1.00    --  -98.50 -80.00  43.82   72
 54  \w   -140.00 -60.00   0.50    1.00    --  -98.50 -77.00  90.00  160
 55  \w   -115.00 -74.00   0.50    0.10    --  -37.97 -57.00  90.00   82
 56  \w   -112.00 -13.00   0.50    0.10    --  -37.97 -77.00 120.00  198
 57  \w   -110.00 -82.00   0.50    0.10    --  -37.97 -57.00  60.00   56
 58  \w   -116.00 -91.00   0.50    0.10    --  -37.97 -77.00 -60.00   50
 59  \w   -147.00 -61.00   0.50    1.00    --  -98.50 -74.00   9.60  172
 60  \w   -138.00 -58.00   0.50    1.00    --  -98.50 -81.00-149.90  160
 61  \w   -132.00 -59.00   0.50    1.00    --  -98.50 -81.00-174.90  146
 62  \w   -139.00 -96.00   0.50    1.00    --  -98.50 -83.00 -24.55   86
 63  \w   -148.00 -59.00   0.50    1.00    --  -98.50 -79.00-137.03  178
 64  \w   -165.00-102.00   0.50    1.00    --  -98.50 -80.00 -38.84  126
 65  \w   -155.00-102.00   0.50    1.00    --  -98.50 -77.00-103.70  106
 66  \w   -170.00 -60.00   0.50    1.00    --  -98.50 -77.00 -60.00  220
 67  \w   -164.00-113.00   0.50    1.00    --  -98.50 -82.00  88.20  102
 68  \w   -169.00 -64.00   0.50    1.00    --  -98.50 -67.00 116.30  210
 69  \w   -170.00 -60.00   0.50    1.00    --  -98.50 -77.00 -90.00  220
 70  \w   -162.00-136.00   0.50    1.00    --  -98.50 -78.00  54.19   52
 71  \w   -177.00 -61.00   0.50    1.00    --  -98.50 -76.00  65.96  232
 72  \w   -169.00-111.00   0.50    1.00    --  -98.50 -77.00-120.00  116
 73  \w   -176.00-144.00   0.50    1.00    --  -98.50 -80.00  43.82   64
 74  \w   -174.00-148.00   0.50    1.00    --  -98.50 -75.00 102.62   52
 75  \w   -174.00 -62.00   0.50    1.00    --  -98.50 -72.00 166.07  224
 76  \w   -176.00-126.00   0.50    1.00    --  -98.50 -77.00 139.45  100
 77  \w   -175.00-147.00   0.50    1.00    --  -98.50 -81.00 119.40   56
 78  \w   -130.00 -41.00   0.50    1.00    --  -98.50 178.00  60.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1546324000
_diffrn_orient_matrix_UB_12      -0.0281544000
_diffrn_orient_matrix_UB_13      0.0132137000
_diffrn_orient_matrix_UB_21      0.0123553000
_diffrn_orient_matrix_UB_22      0.1306157000
_diffrn_orient_matrix_UB_23      0.0562505000
_diffrn_orient_matrix_UB_31      -0.0609608000
_diffrn_orient_matrix_UB_32      0.0754158000
_diffrn_orient_matrix_UB_33      -0.0741240000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31420
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.350
_diffrn_reflns_theta_min         2.696
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.646
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0413P)^2^+0.9534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5801
_reflns_number_total             5980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05578j2.cif
_cod_data_source_block           s1-pe
_cod_depositor_comments
'Adding full bibliography for 7061196--7061202.cif.'
_cod_database_code               7061200
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.899
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C25(H25), C22(H22), C15(H15), C28(H28), C8(H8), C12(H12), C17(H17),
 C16(H16), C34(H34), C6(H6), C23(H23), C2(H2), C38(H38), C32(H32), C29(H29),
 C10(H10), C24(H24), C11(H11), C9(H9), C4(H4), C30(H30), C35(H35), C36(H36),
 C31(H31), C37(H37), C5(H5), C3(H3)
;
_shelx_res_checksum              61540
_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 1.380
_oxdiff_exptl_absorpt_empirical_full_min 0.758