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_7715292
_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
'C62 H52 Cu N2 O P2, F6 P, 0.75(C4 H10 O), 0.375[C4H10O1]'
_chemical_formula_sum            'C66.5 H63.25 Cu F6 N2 O2.13 P3'
_chemical_formula_weight         1194.97
_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     iterative
_audit_creation_date             2022-02-08
_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                85.9700(10)
_cell_angle_beta                 66.9620(10)
_cell_angle_gamma                89.8750(10)
_cell_formula_units_Z            4
_cell_length_a                   18.1906(3)
_cell_length_b                   18.7096(3)
_cell_length_c                   18.9000(3)
_cell_measurement_reflns_used    113723
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.93
_cell_measurement_theta_min      2.64
_cell_volume                     5902.51(17)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
 3646 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI Cu'
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            123971
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.231
_diffrn_reflns_theta_min         2.641
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.837
_exptl_absorpt_correction_T_max  0.4213
_exptl_absorpt_correction_T_min  0.1270
_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    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2485
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.16
_exptl_crystal_size_rad          0.190
_refine_diff_density_max         1.146
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.00355(16)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1428
_refine_ls_number_reflns         22922
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.1074
_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^)+(0.1000P)^2^+23.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2457
_refine_ls_wR_factor_ref         0.2775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15721
_reflns_number_total             22922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           mem146_150k
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_original_formula_sum        'C66.50 H63.25 Cu F6 N2 O2.13 P3'
_cod_database_code               7715292
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.677
_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. Restrained distances
 C126-C125 \\sim C128-C127 \\sim C131-C132 \\sim C130-C129
 with sigma of 0.02
 O3-C125 \\sim O3-C127 \\sim O4-C129 \\sim O4-C131
 with sigma of 0.02
 P6-F3 \\sim P6-F7 \\sim P6-F2 \\sim P6-F9 \\sim P6-F5 \\sim P6-F11
 with sigma of 0.02
 F3-F7 \\sim F3-F2 \\sim F3-F9 \\sim F3-F11 \\sim F7-F2 \\sim F7-F9 \\sim F7-F5
\\sim F2-F5 \\sim F2-F11 \\sim F9-
 F5 \\sim F9-F11 \\sim F5-F11
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C130) = Uanis(C129) = Uanis(C131) = Uanis(C132)
4. Others
 Fixed Sof: O3(0.75) C126(0.75) H12C(0.75) H12D(0.75) H12E(0.75) C125(0.75)
 H12F(0.75) H12G(0.75) C127(0.75) H12H(0.75) H12I(0.75) C128(0.75) H12J(0.75)
 H12K(0.75) H12L(0.75) O4(0.75) C131(0.75) H13A(0.75) H13B(0.75) C132(0.75)
 H13C(0.75) H13D(0.75) H13E(0.75) C129(0.75) H12M(0.75) H12N(0.75) C130(0.75)
 H13F(0.75) H13G(0.75) H13H(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C12(H12A,H12B), C82(H82A,H82B), C73(H73A,H73B), C11(H11A,
 H11B), C19(H19A,H19B), C74(H74A,H74B), C20(H20A,H20B), C125(H12F,H12G),
 C127(H12H,H12I), C131(H13A,H13B), C129(H12M,H12N)
5.b Aromatic/amide H refined with riding coordinates:
 C50(H50), C47(H47), C90(H90), C106(H106), C108(H108), C71(H71), C30(H30),
 C69(H69), C111(H111), C121(H121), C80(H80), C124(H124), C49(H49), C52(H52),
 C40(H40), C123(H123), C105(H105), C43(H43), C32(H32), C84(H84), C79(H79),
 C110(H110), C48(H48), C34(H34), C7(H7), C98(H98), C114(H114), C97(H97),
 C96(H96), C38(H38), C109(H109), C44(H44), C70(H70), C117(H117), C86(H86),
 C66(H66), C104(H104), C42(H42), C94(H94), C14(H14), C100(H100), C122(H122),
 C29(H29), C77(H77), C55(H55), C76(H76), C85(H85), C120(H120), C103(H103),
 C53(H53), C31(H31), C115(H115), C18(H18), C37(H37), C41(H41), C60(H60),
 C58(H58), C56(H56), C99(H99), C118(H118), C116(H116), C8(H8), C65(H65),
 C54(H54), C62(H62), C16(H16), C9(H9), C78(H78), C59(H59), C88(H88), C64(H64),
 C22(H22), C26(H26), C15(H15), C17(H17), C87(H87), C2(H2), C24(H24), C4(H4),
 C25(H25), C23(H23), C3(H3), C93(H93), C92(H92), C91(H91), C36(H36), C35(H35),
 C61(H61)
5.c Idealised Me refined as rotating group:
 C126(H12C,H12D,H12E), C128(H12J,H12K,H12L), C132(H13C,H13D,H13E), C130(H13F,
 H13G,H13H)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4729
_shelx_fab_checksum              55054
_olex2_date_sample_data_collection 2022-02-02
_olex2_date_sample_submission    2022-01-27
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id MEM146_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   5.6
_stoe_evaluation_integration_b   -1.0
_stoe_evaluation_integration_ems 0.011
_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 96.7
_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 146.5
_stoe_evaluation_lana_max_2theta_desired 146.5
_stoe_evaluation_lana_mean_redundancy 5.4
_stoe_evaluation_lana_number_refls_after_or 123971
_stoe_evaluation_lana_number_refls_outliers 27284
_stoe_evaluation_lana_number_refls_total 151255
_stoe_evaluation_lana_number_refls_unique 22922
_stoe_evaluation_lana_number_refls_written 123971
_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          12.6   28.4   44.2   60.0   75.8   91.6  107.4  123.2  139.0
<Resolution>    5.50   2.93   2.01   1.50   1.25   1.08   0.95   0.88   0.83
N(total)         162   2588   6995  16949  30900  33080  22808  25024  12749
<Redundancy>     1.5    2.7    3.4    5.3    7.6    7.0    4.5    5.3    4.1
Complet. [%%]    65.8   99.3  100.0  100.0  100.0   99.8   99.1   98.0   82.0
<I/sigma>      111.4   46.6   25.3   12.9    8.3    5.6    3.4    1.6    0.6
R(int)         0.026  0.038  0.039  0.053  0.064  0.084  0.152  0.339  0.541
;
_stoe_measurement_identifier     MEM146_150K
_stoe_measurement_max_exposure_per_frame '10.0 s'
_stoe_measurement_mean_exposure_per_frame '8.4 s'
_stoe_measurement_min_exposure_per_frame '4.0 s'
_stoe_measurement_total_exposure_time '8.5 h'
_stoe_measurement_total_frame_number 3646
_stoe_measurement_total_run_number 66
_stoe_measurement_tube_power     '50.0 W'