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_7061196
_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 Cu I P2'
_chemical_formula_sum            'C38 H28 Cu I P2'
_chemical_formula_weight         736.98
_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             2019-04-24
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_audit_update_record
;
2021-08-21 deposited with the CCDC.	2022-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                95.271(2)
_cell_angle_beta                 102.089(2)
_cell_angle_gamma                92.733(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4282(3)
_cell_length_b                   10.0360(3)
_cell_length_c                   16.8484(5)
_cell_measurement_reflns_used    11785
_cell_measurement_temperature    241(7)
_cell_measurement_theta_max      29.5550
_cell_measurement_theta_min      2.2430
_cell_volume                     1548.60(8)
_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      241(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.978
_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    -15.00  74.00   0.50    9.59    --    7.96  57.00   0.00  178
  2  \w    -13.00  86.00   0.50    9.59    --    7.96  34.00 -90.00  198
  3  \w    -11.00  44.00   0.50    9.59    --    7.96  57.00-120.00  110
  4  \w    -70.00  15.00   0.50    9.59    --    7.96 -34.00 111.00  170
  5  \w    -26.00  11.00   0.50    9.59    --   -6.48 -99.00  90.00   74
  6  \w    -66.00  30.00   0.50    9.59    --    7.96 -57.00  30.00  192
;
_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      0.0612942000
_diffrn_orient_matrix_UB_12      0.0438044000
_diffrn_orient_matrix_UB_13      0.0191800000
_diffrn_orient_matrix_UB_21      -0.0461207000
_diffrn_orient_matrix_UB_22      0.0531280000
_diffrn_orient_matrix_UB_23      0.0032545000
_diffrn_orient_matrix_UB_31      -0.0079618000
_diffrn_orient_matrix_UB_32      -0.0178913000
_diffrn_orient_matrix_UB_33      0.0386720000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17623
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.043
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.832
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84278
_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    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.369
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0549P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5407
_reflns_number_total             6190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05578j2.cif
_cod_data_source_block           hubu-ll-ln-i
_cod_depositor_comments
'Adding full bibliography for 7061196--7061202.cif.'
_cod_database_code               7061196
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H N O P Cu I'
_diffrn_oxdiff_ac3_digest_frames
;
011c29e75c3e7fc41d31ac703ba0e4c46f00046e99f
;
_diffrn_oxdiff_ac3_digest_hkl
;
01ea468f68d272c019768d2d533aab956e119c
;
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C4(H4), C36(H36), C11(H11), C7(H7), C26(H26), C29(H29), C21(H21),
 C5(H5), C6(H6), C32(H32), C17(H17), C20(H20), C41(H41), C19(H19), C40(H40),
 C38(H38), C15(H15), C35(H35), C28(H28), C34(H34), C27(H27), C18(H18), C33(H33),
  C13(H13), C39(H39), C12(H12), C14(H14)
;
_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 3.622
_oxdiff_exptl_absorpt_empirical_full_min 0.497