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_7715289
_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         'C65 H56 Cu N2 O P2, F6 P'
_chemical_formula_sum            'C65 H56 Cu F6 N2 O P3'
_chemical_formula_weight         1151.56
_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             2022-02-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-01-09 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                83.1420(10)
_cell_angle_beta                 77.5710(10)
_cell_angle_gamma                85.1960(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9248(2)
_cell_length_b                   12.5855(2)
_cell_length_c                   18.3632(3)
_cell_measurement_reflns_used    86531
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.90
_cell_measurement_theta_min      2.48
_cell_volume                     2667.30(8)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)'
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
 3694 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Basel-Cu-Stoe
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50581
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.869
_diffrn_reflns_theta_min         3.544
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.997
_exptl_absorpt_correction_T_max  0.2128
_exptl_absorpt_correction_T_min  0.1504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and Et2O  by solvent layering'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_crystal_size_rad          0.200
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0052(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         10383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1087P)^2^+1.2203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9499
_reflns_number_total             10383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           mem147_150k
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_database_code               7715289
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C55(H55), C51(H51), C53(H53), C44(H44), C52(H52), C2(H2), C45(H45),
 C59(H59), C34(H34), C61(H61), C4(H4), C7(H7), C22(H22), C62(H62), C56(H56),
 C3(H3), C28(H28), C63(H63), C35(H35), C65(H65), C26(H26), C8(H8), C57(H57),
 C38(H38), C9(H9), C58(H58), C23(H23), C14(H14), C36(H36), C32(H32), C15(H15),
 C25(H25), C64(H64), C18(H18), C16(H16), C29(H29), C24(H24), C37(H37), C30(H30),
  C17(H17), C31(H31)
2.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              2668
_olex2_date_sample_data_collection 2022-02-17
_olex2_date_sample_submission    2022-01-18
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id MEM147_150K
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   6.0
_stoe_evaluation_integration_b   -0.4
_stoe_evaluation_integration_ems 0.017
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 97.5
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 145.8
_stoe_evaluation_lana_max_2theta_desired 145.8
_stoe_evaluation_lana_mean_redundancy 4.9
_stoe_evaluation_lana_number_refls_after_or 50586
_stoe_evaluation_lana_number_refls_outliers 11933
_stoe_evaluation_lana_number_refls_total 62519
_stoe_evaluation_lana_number_refls_unique 10386
_stoe_evaluation_lana_number_refls_written 50586
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta          14.0   29.6   45.2   60.8   76.4   92.0  107.6  123.2  138.8
<Resolution>    5.41   2.87   1.97   1.49   1.24   1.07   0.95   0.88   0.83
N(total)         153   1419   3400   7930  13481  14302   9177   8134   4523
<Redundancy>     1.9    3.0    3.6    5.5    7.5    6.8    4.2    3.6    2.7
Complet. [%%]    93.5   99.7  100.0  100.0  100.0   99.6   98.9   98.3   86.1
<I/sigma>      227.7  104.7   59.9   33.7   23.9   19.1   14.8   12.5   10.5
R(int)         0.032  0.021  0.018  0.021  0.022  0.023  0.028  0.055  0.114
;
_stoe_measurement_identifier     MEM147_150K
_stoe_measurement_max_exposure_per_frame '7.0 s'
_stoe_measurement_mean_exposure_per_frame '6.7 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '6.9 h'
_stoe_measurement_total_frame_number 3694
_stoe_measurement_total_run_number 62
_stoe_measurement_tube_power     '50.0 W'