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_7061199
_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         'C40 H32 Cu I O2 P2'
_chemical_formula_sum            'C40 H32 Cu I O2 P2'
_chemical_formula_weight         797.03
_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             2020-09-18
_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                91.4830(10)
_cell_angle_beta                 108.8900(10)
_cell_angle_gamma                113.9130(10)
_cell_formula_units_Z            2
_cell_length_a                   12.13200(10)
_cell_length_b                   12.5512(2)
_cell_length_c                   12.93080(10)
_cell_measurement_reflns_used    18974
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.3300
_cell_measurement_theta_min      3.6540
_cell_volume                     1674.70(4)
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.941
_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      8.00 115.00   0.50    0.34    --   37.97  57.00   0.00  214
  2  \w     90.00 115.00   0.50    0.34    --   37.97  57.00 -90.00   50
  3  \w    101.00 138.00   0.50    1.00    --  112.45 110.00 -62.00   74
  4  \w     81.00 171.00   0.50    1.00    --  112.45  30.00-180.00  180
  5  \w     64.00 112.00   0.50    1.00    --  112.45-111.00 -60.00   96
  6  \w     55.00 112.00   0.50    1.00    --  112.45-110.00-157.00  114
  7  \w     42.00  68.00   0.50    0.34    --   37.97-110.00-157.00   52
  8  \w     31.00  61.00   0.50    1.00    --  112.45-111.00 -60.00   60
  9  \w     27.00 103.00   0.50    1.00    --  112.45 -94.00   0.00  152
 10  \w     40.00  93.00   0.50    1.00    --  112.45 -94.00  30.00  106
 11  \w     57.00  93.00   0.50    1.00    --  112.45 -94.00 120.00   72
 12  \w     27.00  99.00   0.50    1.00    --  112.45 -94.00  90.00  144
 13  \w     12.00  39.00   0.50    0.34    --   37.97  57.00 -90.00   54
 14  \w     41.00  67.00   0.50    0.34    --   37.97  57.00 -90.00   52
 15  \w      5.00 112.00   0.50    0.34    --   37.97  77.00 -60.00  214
 16  \w     61.00 126.00   0.50    0.34    --   37.97 178.00-150.00  130
 17  \w     60.00 126.00   0.50    0.34    --   37.97 178.00 -30.00  132
 18  \w     73.00 113.00   0.50    0.34    --   37.97  57.00 150.00   80
 19  \w      9.00  70.00   0.50    0.34    --   37.97  57.00 150.00  122
 20  \w     -2.00  32.00   0.50    0.34    --   37.97  95.00 -25.57   68
 21  \w    -51.00 -26.00   0.50    0.08    --    0.00 110.00 -62.00   50
 22  \w      8.00 103.00   0.50    0.34    --   37.97  77.00-180.00  190
 23  \w     28.00 108.00   0.50    1.00    --  112.45 -94.00-150.00  160
 24  \w    -48.00 -22.00   0.50    0.34    --  -37.97 110.00 -62.00   52
 25  \w    -58.00  33.00   0.50    0.34    --  -37.97  57.00 -30.00  182
 26  \w    -61.00  -4.00   0.50    0.34    --  -37.97 -77.00  60.00  114
 27  \w    -54.00  -4.00   0.50    0.34    --  -37.97 -77.00  30.00  100
 28  \w    -83.00 -58.00   0.50    1.00    --  -98.50 -81.00  77.27   50
 29  \w    -86.00 -60.00   0.50    1.00    --  -98.50 -77.00  14.44   52
 30  \w    -91.00 -59.00   0.50    1.00    --  -98.50 -79.00  47.06   64
 31  \w    -85.00 -58.00   0.50    1.00    --  -98.50 -82.00 100.75   54
 32  \w    -88.00 -60.00   0.50    1.00    --  -98.50 -77.00  60.00   56
 33  \w    -89.00 -58.00   0.50    1.00    --  -98.50 -83.00   6.39   62
 34  \w    -86.00 -60.00   0.50    1.00    --  -98.50 -79.00 -33.31   52
 35  \w    -89.00 -64.00   0.50    1.00    --  -98.50 -66.00 -91.85   50
 36  \w    -93.00 -60.00   0.50    1.00    --  -98.50 -77.00 -30.00   66
 37  \w    -99.00 -58.00   0.50    1.00    --  -98.50 -82.00  -9.49   82
 38  \w    -92.00 -60.00   0.50    1.00    --  -98.50 -77.00 -98.37   64
 39  \w    -95.00 -60.00   0.50    1.00    --  -98.50 -77.00-176.78   70
 40  \w    -92.00 -62.00   0.50    1.00    --  -98.50 -74.00-134.26   60
 41  \w   -108.00 -60.00   0.50    1.00    --  -98.50 -77.00 -90.00   96
 42  \w   -100.00 -65.00   0.50    0.34    --  -37.97 -77.00  30.00   70
 43  \w   -114.00 -69.00   0.50    0.34    --  -37.97 -77.00  60.00   90
 44  \w   -127.00 -60.00   0.50    1.00    --  -98.50 -77.00  90.00  134
 45  \w    -83.00 -58.00   0.50    1.00    --  -98.50 -82.00 139.80   50
 46  \w    -84.00 -59.00   0.50    1.00    --  -98.50 -80.00 176.33   50
 47  \w   -128.00 -60.00   0.50    1.00    --  -98.50 -77.00 150.00  136
 48  \w   -142.00-102.00   0.50    1.00    --  -98.50 -79.00  47.06   80
 49  \w   -135.00 -59.00   0.50    1.00    --  -98.50 -80.00 122.82  152
 50  \w   -139.00-113.00   0.50    1.00    --  -98.50 -77.00  60.00   52
 51  \w   -138.00-113.00   0.50    1.00    --  -98.50 -77.00  14.44   50
 52  \w   -139.00 -58.00   0.50    1.00    --  -98.50 -83.00  58.81  162
 53  \w   -147.00 -61.00   0.50    1.00    --  -98.50 -74.00 103.72  172
 54  \w    -68.00  32.00   0.50    0.34    --  -37.97  57.00  90.00  200
 55  \w    -83.00 -51.00   0.50    0.34    --  -37.97 110.00 -62.00   64
 56  \w    -79.00 -45.00   0.50    1.00    --  -98.50 110.00 -62.00   68
 57  \w   -120.00 -62.00   0.50    1.00    --  -98.50 -72.00-114.76  116
 58  \w   -149.00-124.00   0.50    1.00    --  -98.50-110.00-157.00   50
 59  \w   -165.00-108.00   0.50    1.00    --  -98.50 -66.00 -91.85  114
 60  \w   -157.00-111.00   0.50    1.00    --  -98.50 -82.00  -9.49   92
 61  \w   -155.00-113.00   0.50    1.00    --  -98.50 -79.00 -33.31   84
 62  \w   -170.00 -98.00   0.50    1.00    --  -98.50 -83.00   6.39  144
 63  \w   -176.00 -60.00   0.50    1.00    --  -98.50 -81.00 168.22  232
 64  \w   -173.00 -62.00   0.50    1.00    --  -98.50 -77.00 -60.00  222
 65  \w   -170.00-135.00   0.50    1.00    --  -98.50 -77.00  90.00   70
 66  \w   -174.00 -60.00   0.50    1.00    --  -98.50 -77.00  30.00  228
 67  \w   -162.00 -60.00   0.50    1.00    --  -98.50 -77.00-150.00  204
 68  \w   -173.00 -98.00   0.50    1.00    --  -98.50 -77.00 -30.00  150
 69  \w   -174.00-114.00   0.50    1.00    --  -98.50 -82.00 100.75  120
 70  \w   -173.00-136.00   0.50    1.00    --  -98.50 -80.00 176.33   74
 71  \w   -174.00-102.00   0.50    1.00    --  -98.50 -82.00 139.80  144
 72  \w   -174.00-142.00   0.50    1.00    --  -98.50 -77.00 150.00   64
 73  \w   -170.00 -61.00   0.50    1.00    --  -98.50 -74.00 -54.50  218
 74  \w   -169.00-144.00   0.50    1.00    --  -98.50 -77.00 -90.00   50
 75  \w   -170.00 -99.00   0.50    1.00    --  -98.50 -77.00 -98.37  142
 76  \w   -169.00 -61.00   0.50    1.00    --  -98.50 -74.00-122.25  216
;
_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      -0.0958574000
_diffrn_orient_matrix_UB_12      -0.1318019000
_diffrn_orient_matrix_UB_13      -0.0432985000
_diffrn_orient_matrix_UB_21      -0.0484669000
_diffrn_orient_matrix_UB_22      0.0270183000
_diffrn_orient_matrix_UB_23      -0.1173339000
_diffrn_orient_matrix_UB_31      0.1036214000
_diffrn_orient_matrix_UB_32      -0.0232636000
_diffrn_orient_matrix_UB_33      -0.0274779000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34129
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.124
_diffrn_reflns_theta_min         3.674
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63801
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.910
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0828P)^2^+0.2420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6257
_reflns_number_total             6405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05578j2.cif
_cod_data_source_block           ln-s3-i
_cod_depositor_comments
'Adding full bibliography for 7061196--7061202.cif.'
_cod_database_code               7061199
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O P Cu'
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.767
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C36(H36), C28(H28), C8(H8), C27(H27), C41(H41), C11(H11), C42(H42),
 C32(H32), C35(H35), C5(H5), C40(H40), C21(H21), C38(H38), C15(H15), C25(H25),
 C34(H34), C20(H20), C33(H33), C26(H26), C14(H14), C12(H12), C13(H13), C18(H18),
  C19(H19), C39(H39)
2.b Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              26471
_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 1.553
_oxdiff_exptl_absorpt_empirical_full_min 0.768