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_7061197
_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 Cl Cu O2 P2'
_chemical_formula_sum            'C40 H32 Cl Cu O2 P2'
_chemical_formula_weight         705.58
_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             2020-08-01
_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                65.047(4)
_cell_angle_beta                 63.653(5)
_cell_angle_gamma                68.840(5)
_cell_formula_units_Z            2
_cell_length_a                   13.3273(7)
_cell_length_b                   13.4397(7)
_cell_length_c                   14.4861(6)
_cell_measurement_reflns_used    7066
_cell_measurement_temperature    295
_cell_measurement_theta_max      27.2190
_cell_measurement_theta_min      4.1590
_cell_volume                     2059.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0353
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.843
_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    -43.00  52.00   1.00   10.36    --  -15.92  77.00  90.00   95
  2  \w    -57.00  -2.00   1.00   10.36    --  -15.92 -57.00-120.00   55
  3  \w    -61.00   1.00   1.00   10.36    --  -15.92 -57.00 -30.00   62
  4  \w    -86.00 -45.00   1.00   10.36    --  -15.92 -19.00 -60.00   41
  5  \w    -18.00  13.00   1.00   10.36    --  -15.92 -19.00 -60.00   31
  6  \w    -11.00  15.00   1.00   10.36    --  -15.92  57.00 -90.00   26
  7  \w     -7.00  76.00   1.00   10.36    --   16.70  77.00-150.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0504750000
_diffrn_orient_matrix_UB_12      -0.0165361000
_diffrn_orient_matrix_UB_13      0.0126941000
_diffrn_orient_matrix_UB_21      0.0334276000
_diffrn_orient_matrix_UB_22      0.0111735000
_diffrn_orient_matrix_UB_23      -0.0559541000
_diffrn_orient_matrix_UB_31      -0.0055852000
_diffrn_orient_matrix_UB_32      0.0561472000
_diffrn_orient_matrix_UB_33      -0.0042449000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18146
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.244
_diffrn_reflns_theta_min         3.305
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         9454
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+0.5833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6935
_reflns_number_total             9454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05578j2.cif
_cod_data_source_block           s3-cl
_cod_depositor_comments
'Adding full bibliography for 7061196--7061202.cif.'
_cod_database_code               7061197
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.972
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Rigid bond restraints
 C19, C20
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.02
 C20, C21
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C20: within 2A with sigma of 0.0008 and sigma for terminal atoms of
0.02
C20 \\sim C21: within 2A with sigma of 0.0008 and sigma for terminal atoms of
0.02
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C4(H4), C1(H1), C3(H3), C2(H2), C34(H34), C13(H13), C40(H40),
 C33(H33), C18(H18), C28(H28), C39(H39), C24(H24), C30(H30), C19(H19), C38(H38),
  C22(H22), C25(H25), C32(H32), C36(H36), C37(H37), C27(H27), C26(H26),
 C31(H31), C20(H20), C21(H21)
4.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              50995
_shelx_fab_checksum              34505
_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 2.149
_oxdiff_exptl_absorpt_empirical_full_min 0.589