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_7715287
_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         'C57 H54 Cu N2 O P2, F6 P, 1.5[C4H10O1]'
_chemical_formula_sum            'C63 H69 Cu F6 N2 O2.5 P3'
_chemical_formula_weight         1164.65
_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             2022-02-11
_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                111.777(2)
_cell_angle_beta                 92.067(2)
_cell_angle_gamma                110.6690(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1185(2)
_cell_length_b                   15.4476(3)
_cell_length_c                   18.7346(4)
_cell_measurement_reflns_used    83428
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.90
_cell_measurement_theta_min      2.59
_cell_volume                     2743.64(11)
_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_detector_type            'DECTRIS EIGER2 1M'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
 3694 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51953
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.336
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.962
_exptl_absorpt_correction_T_max  0.1887
_exptl_absorpt_correction_T_min  0.1040
_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    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1218
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and Et2O  by solvent layering'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.21
_exptl_crystal_size_rad          0.260
_refine_diff_density_max         1.213
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.0070(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   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         10717
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_gt           0.1261
_refine_ls_shift/su_max          0.000
_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^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2600
_refine_ls_wR_factor_ref         0.2708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9265
_reflns_number_total             10717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           mem157_150k
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_original_cell_volume        2743.64(10)
_cod_original_formula_sum        'C63 H69 Cu F6 N2 O2.50 P3'
_cod_database_code               7715287
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.683
_shelx_estimated_absorpt_t_min   0.572
_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
 F1-F6 \\sim F1-F8 \\sim F1-F10 \\sim F1-F5 \\sim F4-F6 \\sim F4-F8 \\sim
F4-F10 \\sim F4-F5 \\sim F6-F8 \\sim F6-
 F5 \\sim F8-F10 \\sim F10-F5
 with sigma of 0.04
 P3-F1 \\sim P3-F4 \\sim P3-F6 \\sim P3-F8 \\sim P3-F10 \\sim P3-F5
 with sigma of 0.02
 F2-F9 \\sim F2-F3 \\sim F9-F7 \\sim F7-F3
 with sigma of 0.04
 P3-F2 \\sim P3-F9 \\sim P3-F1 \\sim P3-F7 \\sim P3-F4 \\sim P3-F3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F10) = Uanis(F5) = Uanis(F8)
Uanis(F3) = Uanis(F2) = Uanis(F9) = Uanis(F7)
4. Others
 Fixed Sof: F6(0.7) F8(0.7) F10(0.7) F5(0.7) F3(0.3) F7(0.3) F2(0.3) F9(0.3)
5.a Ternary CH refined with riding coordinates:
 C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C18(H18A,H18B), C17(H17A,
 H17B), C15(H15A,H15B), C16(H16A,H16B)
5.c Aromatic/amide H refined with riding coordinates:
 C50(H50), C49(H49), C47(H47), C51(H51), C48(H48), C30(H30), C28(H28),
 C36(H36), C53(H53), C3(H3), C37(H37), C10(H10), C35(H35), C29(H29), C7(H7),
 C55(H55), C4(H4), C41(H41), C2(H2), C57(H57), C20(H20), C24(H24), C9(H9),
 C54(H54), C42(H42), C56(H56), C21(H21), C22(H22), C23(H23), C8(H8), C45(H45),
 C43(H43), C44(H44)
5.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32371
_shelx_fab_checksum              3322
_olex2_date_sample_data_collection 2022-02-09
_olex2_date_sample_submission    2022-01-20
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id MEM157_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 0.010
_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 97.2
_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 146.7
_stoe_evaluation_lana_max_2theta_desired 146.7
_stoe_evaluation_lana_mean_redundancy 4.8
_stoe_evaluation_lana_number_refls_after_or 51972
_stoe_evaluation_lana_number_refls_outliers 19127
_stoe_evaluation_lana_number_refls_total 71099
_stoe_evaluation_lana_number_refls_unique 10727
_stoe_evaluation_lana_number_refls_written 51972
_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          12.7   28.5   44.3   60.1   75.9   91.7  107.5  123.3  139.1
<Resolution>    5.60   2.95   2.03   1.50   1.25   1.08   0.95   0.88   0.83
N(total)         136   1543   3523   7482  14767  15262  10314  11695   6377
<Redundancy>     1.8    3.3    3.3    4.5    6.7    6.1    3.9    4.8    3.9
Complet. [%%]    89.0  100.0  100.0  100.0  100.0   99.8   99.1   98.4   84.3
<I/sigma>      425.9  162.8   94.1   45.3   27.8   19.0   11.7    5.0    1.8
R(int)         0.023  0.039  0.043  0.049  0.055  0.059  0.100  0.253  0.387
;
_stoe_measurement_identifier     MEM157_150K
_stoe_measurement_max_exposure_per_frame '5.0 s'
_stoe_measurement_mean_exposure_per_frame '4.9 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '5.0 h'
_stoe_measurement_total_frame_number 3694
_stoe_measurement_total_run_number 62
_stoe_measurement_tube_power     '50.0 W'