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_7061198
_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         'C42 H36 Cu I O4 P2'
_chemical_formula_sum            'C42 H36 Cu I O4 P2'
_chemical_formula_weight         857.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-17
_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
_cell_angle_beta                 94.1760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.33060(10)
_cell_length_b                   16.7868(2)
_cell_length_c                   18.7717(3)
_cell_measurement_reflns_used    11023
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      73.5210
_cell_measurement_theta_min      4.4370
_cell_volume                     3875.26(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      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_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     22.00  51.00   0.50    1.50    --   37.97 -57.00 -60.00   58
  2  \w     30.00  73.00   0.50    1.50    --   37.97-108.00  52.00   86
  3  \w     82.00 108.00   0.50    4.00    --  112.45-108.00  52.00   52
  4  \w    116.00 144.00   0.50    4.00    --  112.45 -61.00  30.00   56
  5  \w     67.00  93.00   0.50    4.00    --  112.45 -61.00  30.00   52
  6  \w     38.00 115.00   0.50    4.00    --  112.45-111.00 -90.00  154
  7  \w     29.00 108.00   0.50    4.00    --  112.45 -94.00  90.00  158
  8  \w     11.00 114.00   0.50    1.50    --   37.97  57.00-120.00  206
  9  \w    103.00 163.00   0.50    4.00    --  112.45 111.00 -90.00  120
 10  \w    100.00 169.00   0.50    4.00    --  112.45 111.00  60.00  138
 11  \w    115.00 178.00   0.50    4.00    --  112.45 108.00 149.00  126
 12  \w     81.00 177.00   0.50    4.00    --  112.45  61.00-150.00  192
 13  \w    -26.00   3.00   0.50    1.21    --    0.00 108.00 149.00   58
 14  \w    -26.00   0.00   0.50    1.50    --   37.97 -57.00 -60.00   52
 15  \w    -23.00  68.00   0.50    1.50    --   37.97 -57.00  30.00  182
 16  \w    -67.00 -42.00   0.50    1.50    --  -37.97 108.00 149.00   50
 17  \w    -88.00 -16.00   0.50    4.00    --  -98.50 108.00 149.00  144
 18  \w    -69.00 -21.00   0.50    4.00    --  -98.50  45.00 -30.00   96
 19  \w    -74.00 -48.00   0.50    4.00    --  -98.50 111.00 -60.00   52
 20  \w    -69.00  46.00   0.50    1.50    --  -37.97  37.00-150.00  230
 21  \w   -125.00-100.00   0.50    4.00    --  -98.50  45.00 -30.00   50
 22  \w   -134.00 -80.00   0.50    4.00    --  -98.50 -94.00-150.00  108
 23  \w   -166.00-140.00   0.50    4.00    --  -98.50 -94.00-150.00   52
 24  \w   -176.00 -82.00   0.50    4.00    --  -98.50 -94.00-180.00  188
 25  \w   -152.00-127.00   0.50    4.00    --  -98.50-108.00  52.00   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      0.0015228000
_diffrn_orient_matrix_UB_12      -0.0171053000
_diffrn_orient_matrix_UB_13      0.0807358000
_diffrn_orient_matrix_UB_21      -0.0289307000
_diffrn_orient_matrix_UB_22      0.0876995000
_diffrn_orient_matrix_UB_23      0.0136185000
_diffrn_orient_matrix_UB_31      -0.1218239000
_diffrn_orient_matrix_UB_32      -0.0209996000
_diffrn_orient_matrix_UB_33      -0.0084673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24047
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.409
_diffrn_reflns_theta_min         3.536
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70028
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+4.0579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7037
_reflns_number_total             7608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05578j2.cif
_cod_data_source_block           exp_4081
_cod_depositor_comments
'Adding full bibliography for 7061196--7061202.cif.'
_cod_database_code               7061198
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C172 H148 Br4 Cu4 O12 P8 '
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.736
_reflns_odcompleteness_completeness 99.99
_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:
 C12(H12), C8(H8), C38(H38), C5(H5), C32(H32), C39(H39), C15(H15), C30(H30),
 C40(H40), C33(H33), C29(H29), C28(H28), C36(H36), C42(H42), C26(H26), C27(H27),
  C24(H24), C41(H41), C23(H23), C34(H34), C35(H35), C20(H20), C22(H22), C21(H21)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C2(H2A,H2B,H2C), C18(H18A,H18B,H18C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              53664
_shelx_fab_checksum              5645
_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 1.887
_oxdiff_exptl_absorpt_empirical_full_min 0.640