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_7061202
_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 Cl Cu P2'
_chemical_formula_sum            'C38 H28 Cl Cu P2'
_chemical_formula_weight         645.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-11-10
_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                94.7320(10)
_cell_angle_beta                 100.9820(10)
_cell_angle_gamma                91.6130(10)
_cell_formula_units_Z            2
_cell_length_a                   9.44320(10)
_cell_length_b                   10.08540(10)
_cell_length_c                   16.6463(2)
_cell_measurement_reflns_used    7761
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.5660
_cell_measurement_theta_min      2.6920
_cell_volume                     1549.47(3)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_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    -21.00  26.00   0.50    0.05    --  -37.97  62.00  74.00   94
  2  \w     -3.00  22.00   0.50    0.05    --    0.00  62.00  74.00   50
  3  \w      6.00 111.00   0.50    0.05    --   37.97  62.00  74.00  210
  4  \w     80.00 128.00   0.50    0.05    --  112.45  62.00  74.00   96
  5  \w     88.00 175.00   0.50    0.05    --  112.45  77.00  90.00  174
  6  \w    143.00 173.00   0.50    0.05    --  112.45 111.00 -90.00   60
  7  \w    100.00 126.00   0.50    0.05    --  112.45 111.00 -90.00   52
  8  \w     83.00 168.00   0.50    0.05    --  112.45  45.00-180.00  170
  9  \w     63.00 114.00   0.50    0.05    --   37.97  57.00-180.00  102
 10  \w     21.00  69.00   0.50    0.05    --   37.97 -62.00 -63.00   96
 11  \w     37.00  80.00   0.50    0.05    --  112.45 -62.00 -63.00   86
 12  \w     77.00 103.00   0.50    0.05    --  112.45 -94.00-120.00   52
 13  \w     34.00 109.00   0.50    0.05    --  112.45-111.00  30.00  150
 14  \w     83.00 108.00   0.50    0.05    --  112.45 -94.00  60.00   50
 15  \w     74.00  99.00   0.50    0.05    --  112.45-111.00  60.00   50
 16  \w     42.00 105.00   0.50    0.05    --  112.45-111.00 150.00  126
 17  \w     40.00  65.00   0.50    0.05    --  112.45 -94.00  60.00   50
 18  \w     30.00  58.00   0.50    0.05    --  112.45-111.00  60.00   56
 19  \w     30.00 114.00   0.50    0.05    --  112.45-111.00 -60.00  168
 20  \w     30.00  56.00   0.50    0.05    --  112.45 -94.00-120.00   52
 21  \w    -28.00  15.00   0.50    0.05    --   37.97 -62.00 -63.00   86
 22  \w    -45.00 -20.00   0.50    0.05    --    0.00 -62.00 -63.00   50
 23  \w   -113.00  -5.00   0.50    0.05    --  -37.97 -62.00 -63.00  216
 24  \w    -54.00 -25.00   0.50    0.05    --  -98.50 111.00 120.00   58
 25  \w    -61.00 -36.00   0.50    0.05    --  -98.50  62.00  74.00   50
 26  \w    -72.00 -24.00   0.50    0.05    --  -98.50 111.00 150.00   96
 27  \w    -71.00 -31.00   0.50    0.05    --  -98.50 111.00  90.00   80
 28  \w    -85.00 -26.00   0.50    0.05    --  -98.50 111.00  60.00  118
 29  \w   -113.00 -88.00   0.50    0.05    --  -98.50  62.00  74.00   50
 30  \w   -162.00 -67.00   0.50    0.05    --  -98.50 -45.00   0.00  190
 31  \w   -118.00 -92.00   0.50    0.05    --  -98.50-111.00  90.00   52
 32  \w   -174.00 -74.00   0.50    0.05    --  -98.50 -62.00 -63.00  200
 33  \w    -89.00 -60.00   0.50    0.05    --    0.00-178.00-180.00   58
 34  \w     27.00  58.00   0.50    0.05    --   37.97  57.00-180.00   62
 35  \w     -3.00  39.00   0.50    0.05    --  -37.97  77.00-180.00   84
 36  \w     62.00 119.00   0.50    0.05    --   37.97 178.00 -60.00  114
 37  \w     68.00 150.00   0.50    0.05    --  112.45 178.00 -60.00  164
 38  \w    -46.00 -15.00   0.50    0.05    --  -98.50 111.00-150.00   62
 39  \w    -76.00 -45.00   0.50    0.05    --  -37.97  77.00-180.00   62
 40  \w    -84.00 -52.00   0.50    0.05    --  -98.50 111.00-150.00   64
 41  \w   -118.00 -41.00   0.50    0.05    --  -98.50 178.00 150.00  154
;
_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      -0.0696924000
_diffrn_orient_matrix_UB_12      0.0666831000
_diffrn_orient_matrix_UB_13      0.0685845000
_diffrn_orient_matrix_UB_21      0.1043919000
_diffrn_orient_matrix_UB_22      0.1224461000
_diffrn_orient_matrix_UB_23      0.0071769000
_diffrn_orient_matrix_UB_31      -0.1091694000
_diffrn_orient_matrix_UB_32      0.0640351000
_diffrn_orient_matrix_UB_33      -0.0648373000
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0285
_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            14868
_diffrn_reflns_theta_full        66.5994
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         2.71
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84248
_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    1.3836
_exptl_crystal_description       block
_exptl_crystal_F_000             663.3993
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.4727
_refine_diff_density_min         -0.4236
_refine_diff_density_rms         0.0570
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             16.2758
_refine_ls_goodness_of_fit_ref   1.0439
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    56
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0439
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.4928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -12
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                5053
_reflns_number_total             5469
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj05578j2.cif
_cod_data_source_block           LN-S1-Cl
_cod_depositor_comments
'Adding full bibliography for 7061196--7061202.cif.'
_cod_database_code               7061202
_chemical_oxdiff_formula         ' C H O Cl P Cu'
_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:
 C10(H10), C6(H6), C7(H7), C41(H41), C4(H4), C5(H5), C14(H14), C20(H20),
 C31(H31), C28(H28), C37(H37), C16(H16), C25(H25), C40(H40), C39(H39), C18(H18),
  C11(H11), C38(H38), C35(H35), C27(H27), C26(H26), C33(H33), C13(H13),
 C19(H19), C34(H34), C12(H12), C32(H32), C17(H17)
;
_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 1.241
_oxdiff_exptl_absorpt_empirical_full_min 0.736