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_7715282
_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
'C54 H42 Cu N2 O P2, F6 P, 0.75(C4 H10 O), 0.4(C H2 Cl2)'
_chemical_formula_sum            'C57.4 H50.3 Cl0.8 Cu F6 N2 O1.75 P3'
_chemical_formula_weight         1094.90
_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   mixed
_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                99.235(2)
_cell_angle_beta                 93.135(2)
_cell_angle_gamma                106.725(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9285(3)
_cell_length_b                   14.8219(4)
_cell_length_c                   19.2356(6)
_cell_measurement_reflns_used    92689
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.63
_cell_measurement_theta_min      2.34
_cell_volume                     2660.53(14)
_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  (Sheldrick, 2015)'
_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 0.984
_diffrn_measured_fraction_theta_max 0.966
_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  0.0202
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42511
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.152
_diffrn_reflns_theta_min         3.168
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.342
_exptl_absorpt_correction_T_max  0.1212
_exptl_absorpt_correction_T_min  0.0843
_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    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             1129
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         9771
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0763
_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^)+(0.1361P)^2^+4.3420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9342
_reflns_number_total             9771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           meme140_150k
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_original_formula_sum        'C57.40 H50.30 Cl0.80 Cu F6 N2 O1.75 P3'
_cod_database_code               7715282
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.570
_shelx_estimated_absorpt_t_min   0.494
_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
 Cl1-C59
 1.78 with sigma of 0.02
 Cl2-C59
 1.77 with sigma of 0.02
 Cl1-C59 = Cl2-C59
 1.771 with sigma of 0.01
 Cl1-Cl2
 2.916 with sigma of 0.03
 C1C-C1D
 1.5 with sigma of 0.02
 O3-C1C
 1.42 with sigma of 0.02
 C1A-C1B
 1.48 with sigma of 0.02
 O3-C1B
 1.41 with sigma of 0.02
 C1B-C1C
 2.3 with sigma of 0.005
 Cl1-Cl2
 2.92 with sigma of 0.04
 O3-C1A = O3-C1D
 2.37 with sigma of 0.04
 O2-C55 \\sim O2-C57
 with sigma of 0.02
 C56-C55 \\sim C58-C57
 with sigma of 0.02
 C1A-O3 \\sim O3-C1D
 with sigma of 0.04
 C1A-C1B \\sim C1C-C1D
 with sigma of 0.02
 O3-C1B \\sim O3-C1C
 with sigma of 0.02
 C1B-C1A \\sim C1D-C1C
 with sigma of 0.02
 O3-C1C \\sim O2-C55 \\sim O2-C57 \\sim O3-C1B
 with sigma of 0.02
 C1B-C1A \\sim C58-C57 \\sim C56-C55 \\sim C1D-C1C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C59: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O3 \\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
Uiso(C56) = Uiso(C55) = Uiso(C57) = Uiso(C58)
Uiso(Cl2) = Uiso(Cl1)
Uanis(F7) = Uanis(F2) = Uanis(F8) = Uanis(F6) = Uanis(F9) = Uanis(F3) =
Uanis(F10) = Uanis(F5)
Uiso(C1A) = Uiso(C1B) = Uiso(C1C) = Uiso(C1D)
4. Rigid body (RIGU) restrains
 Cl1, Cl2, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F6(0.5) F3(0.5) F2(0.5) F5(0.5) C58(0.5) H58A(0.5) H58B(0.5)
 H58C(0.5) O2(0.5) C55(0.5) H55A(0.5) H55B(0.5) C57(0.5) H57A(0.5) H57B(0.5)
 C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) Cl1(0.4) Cl2(0.4) C59(0.4) H59A(0.4)
 H59B(0.4) F7(0.5) F10(0.5) F8(0.5) F9(0.5) O3(0.25) C1A(0.25) H1AA(0.25)
 H1AB(0.25) H1AC(0.25) C1B(0.25) H1BA(0.25) H1BB(0.25) C1C(0.25) H1CA(0.25)
 H1CB(0.25) C1D(0.25) H1DA(0.25) H1DB(0.25) H1DC(0.25)
6.a Riding coordinates:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB,H1DC)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C55(H55A,H55B), C57(H57A,H57B), C59(H59A,H59B)
6.c Aromatic/amide H refined with riding coordinates:
 C44(H44), C10(H10), C50(H50), C48(H48), C9(H9), C7(H7), C42(H42), C39(H39),
 C54(H54), C20(H20), C35(H35), C45(H45), C26(H26), C41(H41), C24(H24), C53(H53),
  C51(H51), C30(H30), C47(H47), C4(H4), C40(H40), C46(H46), C8(H8), C32(H32),
 C21(H21), C34(H34), C22(H22), C52(H52), C2(H2), C27(H27), C33(H33), C23(H23),
 C14(H14), C3(H3), C28(H28), C29(H29), C15(H15), C16(H16)
6.d Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              83439
_olex2_date_sample_submission    2021-07-15
_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 MEM140_150K
_olex2_submission_special_instructions 'No special instructions were received'