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_7715283
_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
'C56 H54 Cu N2 O P2, F6 P, 0.4(C4 H9 O), 0.4(C4 H10 O)'
_chemical_formula_sum            'C59.2 H61.6 Cu F6 N2 O1.8 P3'
_chemical_formula_weight         1100.35
_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             2021-08-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-01-09 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                113.4400(10)
_cell_angle_beta                 90.8650(10)
_cell_angle_gamma                109.8700(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1704(2)
_cell_length_b                   15.2169(3)
_cell_length_c                   18.9218(3)
_cell_measurement_reflns_used    94011
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.50
_cell_measurement_theta_min      2.58
_cell_volume                     2732.78(9)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.90, Darmstadt 2020
;
_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 0.988
_diffrn_measured_fraction_theta_max 0.972
_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  0.0223
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48998
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.264
_diffrn_reflns_theta_min         2.585
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.929
_exptl_absorpt_correction_T_max  0.3659
_exptl_absorpt_correction_T_min  0.2650
_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    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             1146
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.578
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0044(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   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         10128
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+4.0848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1993
_refine_ls_wR_factor_ref         0.2025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9417
_reflns_number_total             10128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           mem139_150k
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_original_formula_sum        'C59.20 H61.60 Cu F6 N2 O1.80 P3'
_cod_database_code               7715283
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.676
_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
 O2-C1B
 1.41 with sigma of 0.02
 O2-C1C
 1.42 with sigma of 0.02
 C1A-C1B
 1.48 with sigma of 0.02
 C1C-C1D
 1.5 with sigma of 0.02
 C1G-C1H
 1.5 with sigma of 0.02
 C1E-C1F
 1.48 with sigma of 0.02
 O3-C1F
 1.41 with sigma of 0.02
 O3-C1G
 1.42 with sigma of 0.02
 O2-C1A = O2-C1D
 2.37 with sigma of 0.04
 O3-C1E = O3-C1H
 2.37 with sigma of 0.04
 C1A-O2 \\sim O2-C1D
 with sigma of 0.04
 O2-C1B \\sim O2-C1C
 with sigma of 0.02
 C1A-C1B \\sim C1C-C1D
 with sigma of 0.02
 C1E-O3 \\sim O3-C1H
 with sigma of 0.04
 C1E-C1F \\sim C1G-C1H
 with sigma of 0.02
 O3-C1F \\sim O3-C1G
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O3 \\sim C1E \\sim C1F \\sim C1G \\sim C1H: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(F10) = Uanis(F2) = Uanis(F9) = Uanis(F3) = Uanis(F8) = Uanis(F6) =
Uanis(F7) = Uanis(F5)
4. Rigid body (RIGU) restrains
 O2, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C1E, C1F, C1G, C1H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F6(0.75) F3(0.75) F2(0.75) F5(0.75) O2(0.4) C1A(0.4) H1AA(0.4)
 H1AB(0.4) H1AC(0.4) C1B(0.4) H1BA(0.4) H1BB(0.4) C1C(0.4) H1C(0.4) C1D(0.4)
 H1DA(0.4) H1DB(0.4) H1DC(0.4) O3(0.4) C1E(0.4) H1EA(0.4) H1EB(0.4) H1EC(0.4)
 C1F(0.4) H1FA(0.4) H1FB(0.4) C1G(0.4) H1GA(0.4) H1GB(0.4) C1H(0.4) H1HA(0.4)
 H1HB(0.4) H1HC(0.4) F7(0.25) F10(0.25) F9(0.25) F8(0.25)
6.a Ternary CH refined with riding coordinates:
 C13(H13)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C1B(H1BA,
 H1BB), C1F(H1FA,H1FB), C1G(H1GA,H1GB)
6.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C23(H23), C41(H41), C39(H39), C31(H31), C22(H22), C52(H52),
 C46(H46), C25(H25), C20(H20), C40(H40), C10(H10), C29(H29), C33(H33), C21(H21),
  C28(H28), C53(H53), C9(H9), C4(H4), C27(H27), C26(H26), C2(H2), C47(H47),
 C8(H8), C32(H32), C7(H7), C50(H50), C56(H56), C3(H3), C54(H54), C48(H48),
 C49(H49), C55(H55), C1C(H1C)
6.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C1A(H1AA,H1AB,H1AC), C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,H1EC), C1H(H1HA,
 H1HB,H1HC)
;
_shelx_res_checksum              10645
_olex2_date_sample_data_collection 2021-08-06
_olex2_date_sample_submission    2021-07-16
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
;
The crystal was mounted on a mylar loop in perfluoroether oil
;
_olex2_submission_original_sample_id MEM139_150K
_olex2_submission_special_instructions 'No special instructions were received'