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_7715286
_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         'C58 H50 Cu N2 O P2, F6 P, 0.8[C4H10O1]'
_chemical_formula_sum            'C61.2 H58 Cu F6 N2 O1.8 P3'
_chemical_formula_weight         1120.74
_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                112.692(2)
_cell_angle_beta                 91.288(3)
_cell_angle_gamma                110.119(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1103(4)
_cell_length_b                   15.0046(5)
_cell_length_c                   18.8034(6)
_cell_measurement_reflns_used    45184
_cell_measurement_temperature    150
_cell_measurement_theta_max      55.77
_cell_measurement_theta_min      2.90
_cell_volume                     2671.60(18)
_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                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
 6888 frames, detector distance = 60 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  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           '1.3401270, 1.34 Ga K\a'
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31586
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         55.644
_diffrn_reflns_theta_min         2.904
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.57
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    3.125
_exptl_absorpt_correction_T_max  0.1675
_exptl_absorpt_correction_T_min  0.0852
_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    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1163
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and Et2O  by solvent layering'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.150
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         10050
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0772
_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^)+(0.0916P)^2^+10.6228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2028
_refine_ls_wR_factor_ref         0.2166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7758
_reflns_number_total             10050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_original_cell_volume        2671.60(17)
_cod_original_formula_sum        'C61.20 H58 Cu F6 N2 O1.80 P3'
_cod_database_code               7715286
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.706
_shelx_estimated_absorpt_t_min   0.619
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-C13 \\sim C20-C13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C24) = Uanis(C23) = Uanis(C21) = Uanis(C25) = Uanis(C22)
Uanis(C14) = Uanis(C18) = Uanis(C17) = Uanis(C15) = Uanis(C19) = Uanis(C16)
4. Others
 Fixed Sof: H13A(0.65) H13B(0.65) H13C(0.35) H13D(0.35) C14(0.65) C15(0.65)
 H15(0.65) C16(0.65) H16(0.65) C17(0.65) H17(0.65) C18(0.65) H18(0.65)
 C19(0.65) H19(0.65) C20(0.35) C21(0.35) H21(0.35) C22(0.35) H22(0.35)
 C23(0.35) H23(0.35) C24(0.35) H24(0.35) C25(0.35) H25(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C13(H13C,H13D)
5.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C28(H28), C31(H31), C10(H10), C41(H41), C43(H43), C7(H7), C29(H29),
 C48(H48), C33(H33), C30(H30), C34(H34), C4(H4), C9(H9), C37(H37), C50(H50),
 C49(H49), C54(H54), C56(H56), C58(H58), C60(H60), C8(H8), C55(H55), C36(H36),
 C61(H61), C35(H35), C64(H64), C57(H57), C42(H42), C2(H2), C3(H3), C62(H62),
 C63(H63), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25)
5.c Fitted hexagon refined as free rotating group:
 C14(C15,C16,C17,C18,C19), C20(C21,C22,C23,C24,C25)
5.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1422
_shelx_fab_checksum              3353
_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 MEM149_150K
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '8.4 cm'
_stoe_detector_size_y            '10.6 cm'
_stoe_evaluation_integration_a   8.0
_stoe_evaluation_integration_b   0.1
_stoe_evaluation_integration_ems 0.014
_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 96.2
_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 111.3
_stoe_evaluation_lana_max_2theta_desired 111.3
_stoe_evaluation_lana_mean_redundancy 3.1
_stoe_evaluation_lana_number_refls_after_or 31603
_stoe_evaluation_lana_number_refls_outliers 8896
_stoe_evaluation_lana_number_refls_total 40499
_stoe_evaluation_lana_number_refls_unique 10059
_stoe_evaluation_lana_number_refls_written 31603
_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          11.4   23.2   35.0   46.8   58.6   70.4   82.2   94.0  105.8
<Resolution>    5.88   3.20   2.20   1.65   1.37   1.16   1.02   0.92   0.85
N(total)         217    647   1388   4162   7476   7156   7589   7315   4549
<Redundancy>     2.5    2.1    2.2    3.5    4.6    3.5    3.3    2.9    2.2
Complet. [%%]   100.0   99.1   99.8   99.5  100.0   99.7   99.3   98.6   83.9
<I/sigma>      213.8  126.7   62.6   31.8   18.1   10.8    6.3    3.9    3.0
R(int)         0.047  0.035  0.042  0.029  0.037  0.045  0.070  0.102  0.136
;
_stoe_measurement_identifier     MEM149_150K
_stoe_measurement_max_exposure_per_frame '12.0 s'
_stoe_measurement_mean_exposure_per_frame '10.1 s'
_stoe_measurement_min_exposure_per_frame '3.0 s'
_stoe_measurement_total_exposure_time '19.3 h'
_stoe_measurement_total_frame_number 6888
_stoe_measurement_total_run_number 44
_stoe_measurement_tube_power     '250 W'