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_7715284
_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         'C57 H48 Cu N2 O P2, 2(F3 P0.5), 0.5(C4 H10 O)'
_chemical_formula_sum            'C59 H53 Cu F6 N2 O1.5 P3'
_chemical_formula_weight         1084.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-10
_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                90
_cell_angle_beta                 115.8860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   47.5822(7)
_cell_length_b                   10.7647(2)
_cell_length_c                   23.4775(4)
_cell_measurement_reflns_used    134387
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.45
_cell_measurement_theta_min      2.09
_cell_volume                     10818.8(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.983
_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  0.0323
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            81904
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.249
_diffrn_reflns_theta_min         5.420
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.940
_exptl_absorpt_correction_T_max  0.6387
_exptl_absorpt_correction_T_min  0.5013
_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    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             4488
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.00018(3)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         10139
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0728
_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^)+(0.1217P)^2^+33.5681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9740
_reflns_number_total             10139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00276h2.cif
_cod_data_source_block           mem141_150k
_cod_depositor_comments
'Adding full bibliography for 7715280--7715292.cif.'
_cod_original_formula_sum        'C59 H53 Cu F6 N2 O1.50 P3'
_cod_database_code               7715284
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.698
_shelx_estimated_absorpt_t_min   0.594
_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-C60 \\sim O2-C58
 with sigma of 0.02
 C59-C58 \\sim C60-C61
 with sigma of 0.02
 P4-F5 \\sim P4-F9 \\sim P4-F8 \\sim P4-F7 \\sim P4-F4
 with sigma of 0.02
 F5-F9 \\sim F5-F8 \\sim F5-F7 \\sim F9-F4 \\sim F8-F7
 with sigma of 0.04
 P4-F6 \\sim P4-F5 \\sim P4-F4 \\sim P4-F9 \\sim P4-F8 \\sim P4-F7
 with sigma of 0.02
 F6-F5 \\sim F6-F4 \\sim F6-F9 \\sim F6-F7 \\sim F5-F9 \\sim F5-F8 \\sim F5-F7
\\sim F4-F9 \\sim F4-F8 \\sim F4-F7
 \\sim F9-F8 \\sim F8-F7
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C59) = Uanis(C58) = Uanis(C60) = Uanis(C61)
4. Others
 Fixed Sof: O2(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C60(0.5) H60A(0.5)
 H60B(0.5) C58(0.5) H58A(0.5) H58B(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
 F5(0.5) F4(0.5) F8(0.5) F7(0.5) F9(0.5) F6(0.5)
5.a Riding coordinates:
 C60(H60A,H60B), C58(H58A,H58B)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B)
5.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C41(H41), C20(H20), C47(H47), C53(H53), C26(H26), C35(H35),
 C51(H51), C34(H34), C10(H10), C30(H30), C4(H4), C39(H39), C24(H24), C54(H54),
 C40(H40), C9(H9), C27(H27), C50(H50), C57(H57), C55(H55), C7(H7), C49(H49),
 C48(H48), C2(H2), C8(H8), C22(H22), C28(H28), C23(H23), C21(H21), C29(H29),
 C3(H3), C56(H56), C15(H15), C14(H14), C16(H16), C18(H18), C17(H17)
5.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C44(H44A,H44B,H44C), C61(H61A,H61B,H61C), C59(H59A,H59B,
 H59C)
;
_shelx_res_checksum              3726
_olex2_date_sample_data_collection 2021-08-09
_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 MEM141_150K
_olex2_submission_special_instructions 'No special instructions were received'