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_7061201
_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 Br Cu O2 P2'
_chemical_formula_sum            'C40 H32 Br Cu O2 P2'
_chemical_formula_weight         750.04
_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             2020-09-02
_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                90.6640(10)
_cell_angle_beta                 114.373(2)
_cell_angle_gamma                108.705(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1192(2)
_cell_length_b                   12.5675(3)
_cell_length_c                   12.6953(2)
_cell_measurement_reflns_used    15757
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0330
_cell_measurement_theta_min      3.7290
_cell_volume                     1644.87(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.937
_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  46.00   0.50    1.74    --   37.97  57.00 -30.00   76
  2  \w     49.00 110.00   0.50    1.74    --   37.97  57.00 -30.00  122
  3  \w     60.00 115.00   0.50    1.74    --   37.97  57.00 -90.00  110
  4  \w    134.00 160.00   0.50    1.74    --  112.45 109.00 -80.00   52
  5  \w     77.00 124.00   0.50    1.74    --   37.97 178.00-150.00   94
  6  \w     60.00 126.00   0.50    1.74    --   37.97 178.00 -60.00  132
  7  \w     75.00 177.00   0.50    1.74    --  112.45  77.00-150.00  204
  8  \w     67.00  92.00   0.50    1.74    --   37.97-109.00-176.00   50
  9  \w     28.00  55.00   0.50    1.74    --   37.97-109.00-176.00   54
 10  \w     67.00 108.00   0.50    1.74    --  112.45-109.00-176.00   82
 11  \w     65.00 106.00   0.50    1.74    --  112.45 -94.00 -90.00   82
 12  \w     49.00 105.00   0.50    1.74    --  112.45 -94.00   0.00  112
 13  \w     32.00 115.00   0.50    1.74    --  112.45-111.00 150.00  166
 14  \w     28.00 105.00   0.50    1.74    --  112.45 -94.00  60.00  154
 15  \w     31.00 108.00   0.50    1.74    --  112.45 -94.00 -60.00  154
 16  \w     34.00  59.00   0.50    1.74    --  112.45 -94.00 -90.00   50
 17  \w     33.00  95.00   0.50    1.74    --  112.45 -94.00-120.00  124
 18  \w     14.00  40.00   0.50    1.74    --   37.97  57.00 -90.00   52
 19  \w      6.00  37.00   0.50    1.74    --   37.97  94.00 -98.34   62
 20  \w      8.00 111.00   0.50    1.74    --   37.97  57.00-150.00  206
 21  \w     12.00 111.00   0.50    1.74    --   37.97  77.00   0.00  198
 22  \w     42.00  68.00   0.50    1.74    --   37.97  57.00 150.00   52
 23  \w     83.00 115.00   0.50    1.74    --   37.97  57.00 150.00   64
 24  \w      8.00  83.00   0.50    1.74    --   37.97  57.00 120.00  150
 25  \w     -5.00  41.00   0.50    1.74    --   37.97  90.00 177.01   92
 26  \w    -65.00  38.00   0.50    1.74    --  -37.97  57.00  90.00  206
 27  \w    -54.00 -29.00   0.50    0.43    --    0.00 109.00 -80.00   50
 28  \w    -48.00 -10.00   0.50    1.74    --  -37.97 109.00 -80.00   76
 29  \w    -62.00  39.00   0.50    1.74    --  -37.97  57.00 -30.00  202
 30  \w    -60.00  -2.00   0.50    1.74    --  -37.97 -77.00  60.00  116
 31  \w    -52.00  -1.00   0.50    1.74    --  -37.97 -77.00 -60.00  102
 32  \w    -84.00 -58.00   0.50    1.74    --  -98.50 -83.00 -19.14   52
 33  \w    -90.00 -60.00   0.50    1.74    --  -98.50 -77.00 -90.00   60
 34  \w    -85.00 -58.00   0.50    1.74    --  -98.50 -83.00-128.82   54
 35  \w    -87.00 -60.00   0.50    1.74    --  -98.50 -77.00-150.00   54
 36  \w    -88.00 -60.00   0.50    1.74    --  -98.50 -77.00-120.00   56
 37  \w    -93.00 -60.00   0.50    1.74    --  -98.50 -77.00-180.00   66
 38  \w   -113.00 -88.00   0.50    1.74    --  -37.97 -77.00 -60.00   50
 39  \w   -143.00-115.00   0.50    1.74    --  -98.50-109.00-176.00   56
 40  \w   -139.00-112.00   0.50    1.74    --  -98.50 -77.00-180.00   54
 41  \w   -130.00 -60.00   0.50    1.74    --  -98.50 -77.00 -98.40  140
 42  \w   -104.00 -58.00   0.50    1.74    --  -98.50 -83.00 -39.38   92
 43  \w    -98.00 -63.00   0.50    1.74    --  -98.50 -70.00  35.43   70
 44  \w    -83.00 -58.00   0.50    1.74    --  -98.50 -83.00  85.56   50
 45  \w    -83.00 -58.00   0.50    1.74    --  -98.50 -81.00 113.98   50
 46  \w    -85.00 -60.00   0.50    1.74    --  -98.50 -77.00  60.00   50
 47  \w    -88.00 -61.00   0.50    1.74    --  -98.50 -74.00 135.65   54
 48  \w    -84.00 -58.00   0.50    1.74    --  -98.50 -82.00 167.07   52
 49  \w    -95.00 -60.00   0.50    1.74    --  -98.50 -77.00  90.00   70
 50  \w   -109.00 -60.00   0.50    1.74    --  -98.50 -77.00  30.00   98
 51  \w   -115.00 -60.00   0.50    1.74    --  -98.50 -77.00   5.04  110
 52  \w   -116.00 -79.00   0.50    1.74    --  -37.97 -77.00  60.00   74
 53  \w   -129.00 -59.00   0.50    1.74    --  -98.50 -79.00 -75.98  140
 54  \w   -134.00 -61.00   0.50    1.74    --  -98.50 -74.00 -16.41  146
 55  \w   -155.00-129.00   0.50    1.74    --  -98.50 -82.00 167.07   52
 56  \w   -123.00 -60.00   0.50    1.74    --  -98.50 -78.00 173.17  126
 57  \w   -150.00 -62.00   0.50    1.74    --  -98.50 -72.00 144.15  176
 58  \w   -157.00-131.00   0.50    1.74    --  -98.50 -77.00  90.00   52
 59  \w   -161.00 -63.00   0.50    1.74    --  -98.50 -70.00 116.58  196
 60  \w   -151.00 -63.00   0.50    1.74    --  -98.50 -71.00  64.29  176
 61  \w   -171.00-126.00   0.50    1.74    --  -98.50 -83.00 -39.38   90
 62  \w   -170.00-118.00   0.50    1.74    --  -98.50 -70.00  35.43  104
 63  \w   -158.00-133.00   0.50    1.74    --  -98.50 -81.00 113.98   50
 64  \w   -177.00-151.00   0.50    1.74    --  -98.50 -78.00 173.17   52
 65  \w   -174.00-107.00   0.50    1.74    --  -98.50 -83.00  85.56  134
 66  \w   -162.00-132.00   0.50    1.74    --  -98.50 -77.00   5.04   60
 67  \w   -167.00-102.00   0.50    1.74    --  -98.50 -83.00 -19.14  130
 68  \w   -171.00 -62.00   0.50    1.74    --  -98.50 -73.00  12.64  218
 69  \w   -176.00-113.00   0.50    1.74    --  -98.50 -83.00-128.82  126
 70  \w   -176.00 -60.00   0.50    1.74    --  -98.50 -78.00 -64.86  232
 71  \w   -167.00 -58.00   0.50    1.74    --  -98.50 -82.00 106.04  218
 72  \w   -176.00-105.00   0.50    1.74    --  -98.50 -77.00  60.00  142
 73  \w   -163.00-104.00   0.50    1.74    --  -98.50 -74.00 135.65  118
 74  \w   -175.00-114.00   0.50    1.74    --  -98.50 -77.00  30.00  122
 75  \w   -174.00-147.00   0.50    1.74    --  -98.50 -77.00 -98.40   54
 76  \w   -177.00-106.00   0.50    1.74    --  -98.50 -77.00-150.00  142
 77  \w   -127.00 -61.00   0.50    1.74    --  -98.50 -75.00 -37.94  132
 78  \w   -163.00-103.00   0.50    1.74    --  -98.50 -77.00-120.00  120
 79  \w   -172.00 -62.00   0.50    1.74    --  -98.50 -73.00-164.63  220
 80  \w    -74.00 -49.00   0.50    1.74    --  -98.50 109.00 -80.00   50
;
_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      0.0933141000
_diffrn_orient_matrix_UB_12      0.0797287000
_diffrn_orient_matrix_UB_13      0.1182367000
_diffrn_orient_matrix_UB_21      0.0286178000
_diffrn_orient_matrix_UB_22      0.1001170000
_diffrn_orient_matrix_UB_23      -0.0653446000
_diffrn_orient_matrix_UB_31      -0.1131384000
_diffrn_orient_matrix_UB_32      0.0291342000
_diffrn_orient_matrix_UB_33      0.0025373000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_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            33367
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.354
_diffrn_reflns_theta_min         3.766
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74626
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0449P)^2^+1.5536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5788
_reflns_number_total             6283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05578j2.cif
_cod_data_source_block           exp_4148-liuli-1
_cod_depositor_comments
'Adding full bibliography for 7061196--7061202.cif.'
_cod_original_cell_volume        1644.87(6)
_cod_database_code               7061201
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O P Br Cu'
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.901
_reflns_odcompleteness_completeness 99.95
_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:
 C5(H5), C28(H28), C8(H8), C32(H32), C17(H17), C36(H36), C42(H42), C11(H11),
 C27(H27), C25(H25), C15(H15), C34(H34), C21(H21), C33(H33), C41(H41), C14(H14),
  C19(H19), C26(H26), C38(H38), C13(H13), C35(H35), C20(H20), C12(H12),
 C18(H18), C40(H40), C39(H39)
2.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              91272
_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 1.364
_oxdiff_exptl_absorpt_empirical_full_min 0.766