Introducing sterically demanding substituents and π-π-interactions into [Cu(P^P)(N^N)]<sup>+</sup> complexes.
Meyer, Marco; Prescimone, Alessandro; Constable, Edwin C.; Housecroft, Catherine E.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5453–5465; doi:10.1039/d4dt00276h

data_7715285
_publ_section_title
;
 Introducing sterically demanding substituents and
 &#x3c0;-&#x3c0;-interactions into [Cu(P^P)(N^N)]<sup>+</sup> complexes.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5453
_journal_page_last               5465
_journal_paper_doi               10.1039/d4dt00276h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C64 H56 Cu N2 O P2, 2(F3 P0.5)'
_chemical_formula_sum            'C64 H56 Cu F6 N2 O P3'
_chemical_formula_weight         1139.55
_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             2022-09-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-09 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                78.071(2)
_cell_angle_beta                 80.439(2)
_cell_angle_gamma                67.579(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1961(2)
_cell_length_b                   13.9132(3)
_cell_length_c                   19.7956(4)
_cell_measurement_reflns_used    29650
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2900
_cell_measurement_theta_min      1.8550
_cell_volume                     2775.96(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.952
_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    -74.00 110.00   0.50   16.00    --   20.00  54.00-120.00  368
  2  \w    -74.00 110.00   0.50   16.00    --   20.00  54.00 150.00  368
  3  \w    -74.00 110.00   0.50   16.00    --   20.00  54.00  30.00  368
  4  \w    -74.00 110.00   0.50   16.00    --   20.00  54.00 -30.00  368
  5  \w    -74.00 110.00   0.50   16.00    --   20.00  54.00  90.00  368
  6  \w    -74.00 110.00   0.50   16.00    --   20.00  54.00 -90.00  368
  7  \w    -74.00 110.00   0.50   16.00    --   20.00  54.00   0.00  368
  8  \w    -74.00  64.00   0.50   16.00    --   20.00  54.00 120.00  276
  9  \w    -74.00 110.00   0.50   16.00    --   20.00  54.00-180.00  368
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0315525000
_diffrn_orient_matrix_UB_12      0.0166465000
_diffrn_orient_matrix_UB_13      -0.0308882000
_diffrn_orient_matrix_UB_21      -0.0611944000
_diffrn_orient_matrix_UB_22      0.0133986000
_diffrn_orient_matrix_UB_23      0.0199378000
_diffrn_orient_matrix_UB_31      -0.0007373000
_diffrn_orient_matrix_UB_32      0.0515940000
_diffrn_orient_matrix_UB_33      -0.0014749000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            78218
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.409
_diffrn_reflns_theta_min         1.776
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.533
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.363
_exptl_crystal_description       plate
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.824
_exptl_crystal_size_mid          0.678
_exptl_crystal_size_min          0.183
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         15998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0527P)^2^+0.7685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12256
_reflns_number_total             15998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           mem150_jmw3108
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_database_code               7715285
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C64 H56 Cu1 F6 N2 O1 P3'
_chemical_oxdiff_usercomment     'crystallized from CHCl2, Et2O'
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.662
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C15(H15), C51(H51), C43(H43), C54(H54), C36(H36), C50(H50),
 C46(H46), C9(H9), C30(H30), C44(H44), C16(H16), C58(H58), C40(H40), C55(H55),
 C49(H49), C2(H2), C4(H4), C7(H7), C56(H56), C45(H45), C57(H57), C60(H60),
 C64(H64), C37(H37), C32(H32), C34(H34), C8(H8), C62(H62), C3(H3), C17(H17),
 C38(H38), C61(H61), C24(H24), C33(H33), C31(H31), C63(H63), C25(H25), C39(H39),
  C26(H26), C19(H19), C28(H28), C18(H18), C27(H27)
;
_shelx_res_checksum              47483
_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 1.336
_oxdiff_exptl_absorpt_empirical_full_min 0.789