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_7715291
_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         'C52 H72 Cu N4, F6 P'
_chemical_formula_sum            'C52 H72 Cu F6 N4 P'
_chemical_formula_weight         961.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-23
_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                 90.068(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0492(4)
_cell_length_b                   12.3630(2)
_cell_length_c                   27.1473(7)
_cell_measurement_reflns_used    123535
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.14
_cell_measurement_theta_min      2.94
_cell_volume                     5050.8(2)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
 3952 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  0.0488
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            104207
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.797
_diffrn_reflns_theta_min         2.936
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.406
_exptl_absorpt_correction_T_max  0.5781
_exptl_absorpt_correction_T_min  0.3814
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and acetone  by solvent layering'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.210
_refine_diff_density_max         0.676
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00141(9)
_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   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         9998
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0882
_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^)+(0.0500P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1794
_refine_ls_wR_factor_ref         0.1961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8147
_reflns_number_total             9998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           mem158_omol_150k
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_database_code               7715291
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.747
_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
2. Uiso/Uaniso restraints and constraints
C48 \\sim C51 \\sim C49 \\sim C52 \\sim C50: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C53 \\sim C55 \\sim C57 \\sim C54 \\sim C56: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C48, C51, C49, C52, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C55, C57, C54, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H46A(0.65) H46B(0.65) H46C(0.35) H46D(0.35) C47(0.65) H47(0.65)
 C48(0.65) H48A(0.65) H48B(0.65) C52(0.65) H52A(0.65) H52B(0.65) C50(0.65)
 H50A(0.65) H50B(0.65) C49(0.65) H49A(0.65) H49B(0.65) C51(0.65) H51A(0.65)
 H51B(0.65) C53(0.35) H53A(0.35) H53B(0.35) C54(0.35) H54A(0.35) H54B(0.35)
 C56(0.35) H56A(0.35) H56B(0.35) C57(0.35) H57A(0.35) H57B(0.35) C55(0.35)
 H55A(0.35) H55B(0.35) C58(0.35) H58(0.35)
5.a Riding coordinates:
 C46(H46A,H46B), C46(H46C,H46D), C47(H47), C57(H57A,H57B), C58(H58)
5.b Ternary CH refined with riding coordinates:
 C21(H21), C39(H39), C13(H13)
5.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C20(H20A,H20B), C19(H19A,H19B), C37(H37A,H37B), C45(H45A,
 H45B), C12(H12A,H12B), C38(H38A,H38B), C40(H40A,H40B), C22(H22A,H22B),
 C44(H44A,H44B), C26(H26A,H26B), C23(H23A,H23B), C14(H14A,H14B), C41(H41A,H41B),
  C18(H18A,H18B), C25(H25A,H25B), C24(H24A,H24B), C43(H43A,H43B), C42(H42A,
 H42B), C15(H15A,H15B), C17(H17A,H17B), C16(H16A,H16B), C48(H48A,H48B),
 C52(H52A,H52B), C50(H50A,H50B), C49(H49A,H49B), C51(H51A,H51B), C53(H53A,H53B),
  C54(H54A,H54B), C56(H56A,H56B), C55(H55A,H55B)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C9(H9), C3(H3), C8(H8), C2(H2), C33(H33), C30(H30), C28(H28),
 C35(H35), C34(H34), C29(H29)
;
_shelx_res_checksum              16838
_olex2_date_sample_data_collection 2022-09-22
_olex2_date_sample_submission    2022-09-05
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id MEM158
_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 0.017
_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 99.3
_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 145.7
_stoe_evaluation_lana_max_2theta_desired 145.7
_stoe_evaluation_lana_mean_redundancy 10.4
_stoe_evaluation_lana_number_refls_after_or 104238
_stoe_evaluation_lana_number_refls_outliers 28070
_stoe_evaluation_lana_number_refls_total 132308
_stoe_evaluation_lana_number_refls_unique 10003
_stoe_evaluation_lana_number_refls_written 104238
_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          13.3   28.9   44.5   60.1   75.7   91.3  106.9  122.5  138.1
<Resolution>    5.45   2.94   2.01   1.49   1.25   1.08   0.95   0.88   0.83
N(total)         283   1704   4895  14233  26569  29124  21416  22358  11726
<Redundancy>     2.9    4.1    5.5   10.5   15.1   14.1    9.1   10.4    6.9
Complet. [%%]    97.1  100.0  100.0  100.0  100.0  100.0  100.0  100.0   95.5
<I/sigma>      251.4   79.1   44.9   23.1   15.6   10.1    6.7    3.7    1.9
R(int)         0.020  0.032  0.032  0.039  0.042  0.053  0.105  0.245  0.374
;
_stoe_measurement_identifier     MEM158_omol_150K
_stoe_measurement_max_exposure_per_frame '6.0 s'
_stoe_measurement_mean_exposure_per_frame '5.9 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '6.4 h'
_stoe_measurement_total_frame_number 3952
_stoe_measurement_total_run_number 37
_stoe_measurement_tube_power     '50.0 W'