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_7715290
_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         'C55 H46 Cu N2 O P2, F6 P'
_chemical_formula_sum            'C55 H46 Cu F6 N2 O P3'
_chemical_formula_weight         1021.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 95.071(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6732(3)
_cell_length_b                   16.9223(4)
_cell_length_c                   29.1542(9)
_cell_measurement_reflns_used    31183
_cell_measurement_temperature    150
_cell_measurement_theta_max      55.90
_cell_measurement_theta_min      2.63
_cell_volume                     4753.7(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
 3593 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           'Ga K\a'
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.1478
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            47843
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         55.747
_diffrn_reflns_theta_min         2.629
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.57
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    3.469
_exptl_absorpt_correction_T_max  0.3170
_exptl_absorpt_correction_T_min  0.0128
_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    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and acetone  by solvent layering'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_size_rad          0.160
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0749
_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^)+(0.1331P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.2099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5706
_reflns_number_total             9089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           mem148_150k
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_database_code               7715290
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.624
_shelx_estimated_absorpt_t_min   0.574
_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), C13(H13A,H13B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C21(H21), C9(H9), C44(H44), C27(H27), C35(H35), C31(H31), C25(H25),
 C38(H38), C41(H41), C48(H48), C10(H10), C53(H53), C54(H54), C7(H7), C52(H52),
 C24(H24), C50(H50), C43(H43), C30(H30), C36(H36), C47(H47), C8(H8), C2(H2),
 C15(H15), C37(H37), C4(H4), C3(H3), C29(H29), C28(H28), C23(H23), C56(H56),
 C49(H49), C19(H19), C42(H42), C16(H16), C55(H55), C22(H22), C17(H17), C18(H18)
;
_shelx_res_checksum              38032
_olex2_date_sample_data_collection 2022-08-29
_olex2_date_sample_submission    2022-08-29
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id MEM148_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 97.7
_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 111.5
_stoe_evaluation_lana_max_2theta_desired 111.5
_stoe_evaluation_lana_mean_redundancy 5.3
_stoe_evaluation_lana_number_refls_after_or 47846
_stoe_evaluation_lana_number_refls_outliers 9339
_stoe_evaluation_lana_number_refls_total 57185
_stoe_evaluation_lana_number_refls_unique 9092
_stoe_evaluation_lana_number_refls_written 47846
_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 2/m
_stoe_evaluation_lana_table
;
2Theta          10.3   22.3   34.3   46.3   58.3   70.3   82.3   94.3  106.3
<Resolution>    6.38   3.29   2.23   1.65   1.37   1.16   1.02   0.92   0.85
N(total)         109    487   1076   4269  10319  10809  11669  11329   7118
<Redundancy>     2.0    2.0    2.2    4.4    7.6    6.5    5.9    5.2    3.8
Complet. [%%]    95.6   94.5   97.6   99.5  100.0  100.0  100.0   99.7   90.4
<I/sigma>       93.6   56.2   23.4   11.7    6.8    4.0    2.3    1.6    1.3
R(int)         0.023  0.035  0.045  0.092  0.101  0.136  0.215  0.289  0.340
;
_stoe_measurement_identifier     MEM148_150K
_stoe_measurement_max_exposure_per_frame '15.0 s'
_stoe_measurement_mean_exposure_per_frame '13.9 s'
_stoe_measurement_min_exposure_per_frame '8.0 s'
_stoe_measurement_total_exposure_time '13.8 h'
_stoe_measurement_total_frame_number 3593
_stoe_measurement_total_run_number 28
_stoe_measurement_tube_power     '250 W'