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_7715280
_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 H52 Cu N2 O P2, F6 P, 0.75(C4 H10 O), 0.5(H2 O)'
_chemical_formula_sum            'C59 H60.5 Cu F6 N2 O2.25 P3'
_chemical_formula_weight         1104.04
_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             2021-04-09
_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                76.289(2)
_cell_angle_beta                 81.110(2)
_cell_angle_gamma                70.345(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9048(2)
_cell_length_b                   16.0127(4)
_cell_length_c                   17.4940(4)
_cell_measurement_reflns_used    81113
_cell_measurement_temperature    150
_cell_measurement_theta_max      57.09
_cell_measurement_theta_min      2.27
_cell_volume                     2785.40(11)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_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  'Olex2 1.3 (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 0.985
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\f and \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           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38847
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         56.640
_diffrn_reflns_theta_min         2.269
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.995
_exptl_absorpt_correction_T_max  0.2912
_exptl_absorpt_correction_T_min  0.0355
_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    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             1149
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         10854
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0548
_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^)+(0.1097P)^2^+2.3005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10577
_reflns_number_total             10854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           mem124_150k
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_original_cell_volume        2785.40(12)
_cod_original_formula_sum        'C59 H60.50 Cu F6 N2 O2.25 P3'
_cod_database_code               7715280
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.586
_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, All O(H,H) groups
2. Restrained distances
 C61-C58
 1.5 with sigma of 0.02
 C65-C57
 1.5 with sigma of 0.005
 C61-C58 \\sim C60-C59
 with sigma of 0.02
 O3-C65 \\sim O3-C63 \\sim O2-C59 \\sim O2-C58
 with sigma of 0.02
 C61-C58 \\sim C60-C59 \\sim C64-C63 \\sim C65-C57
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C60) = Uanis(C59) = Uanis(O2) = Uanis(C58) = Uanis(C61)
Uanis(C64) = Uanis(C63) = Uanis(O3) = Uanis(C65) = Uanis(C57)
4. Others
 Fixed Sof: O2(0.5) C59(0.5) H59A(0.5) H59B(0.5) C58(0.5) H58A(0.5) H58B(0.5)
 C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
 C64(0.25) H64A(0.25) H64B(0.25) H64C(0.25) C63(0.25) H63A(0.25) H63B(0.25)
 C65(0.25) H65A(0.25) H65B(0.25) O3(0.25) O4(0.25) H4A(0.25) H4B(0.25)
 C57(0.25) H57A(0.25) H57B(0.25) H57C(0.25) O5(0.25) H5A(0.25) H5B(0.25)
5.a Riding coordinates:
 C59(H59A,H59B), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), O4(H4A), O4(H4B),
 C57(H57A,H57B,H57C), O5(H5A), O5(H5B)
5.b Ternary CH refined with riding coordinates:
 C11(H11)
5.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C15(H15A,H15B), C13(H13A,
 H13B), C58(H58A,H58B), C63(H63A,H63B), C65(H65A,H65B)
5.d Aromatic/amide H refined with riding coordinates:
 C40(H40), C32(H32), C31(H31), C33(H33), C41(H41), C46(H46), C50(H50),
 C47(H47), C52(H52), C25(H25), C42(H42), C7(H7), C48(H48), C4(H4), C49(H49),
 C2(H2), C9(H9), C19(H19), C56(H56), C8(H8), C53(H53), C23(H23), C29(H29),
 C55(H55), C54(H54), C26(H26), C3(H3), C20(H20), C22(H22), C21(H21), C27(H27),
 C28(H28)
5.e Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C17(H17A,H17B,H17C), C43(H43A,H43B,H43C), C61(H61A,H61B,
 H61C)
;
_shelx_res_checksum              21281
_olex2_date_sample_data_collection 2021-04-08
_olex2_date_sample_submission    2021-03-22
_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 MEM124_150K
_olex2_submission_special_instructions 'No special instructions were received'