Introducing intramolecular, interligand arene–alkynyl π-interactions into heteroleptic [Cu(N^N)(P^P)]+ complexes
Gejsnæs-Schaad, Deyanira; Meyer, Marco; Prescimone, Alessandro; Housecroft, Catherine E.; Constable, Edwin C.; CrystEngComm 25 (2023) 3000–3012; doi:10.1039/D3CE00355H

data_7246704
_publ_section_title
;
 Introducing intramolecular, interligand arene--alkynyl \p-interactions
 into heteroleptic [Cu(N^N)(P^P)]+ complexes
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              3000
_journal_page_last               3012
_journal_paper_doi               10.1039/D3CE00355H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C57 H48 Cu N2 O P2, F6 P'
_chemical_formula_sum            'C57 H48 Cu F6 N2 O P3'
_chemical_formula_weight         1047.42
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-08 deposited with the CCDC.	2023-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.5210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0919(3)
_cell_length_b                   14.2952(3)
_cell_length_c                   20.6426(3)
_cell_measurement_reflns_used    100343
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.35
_cell_measurement_theta_min      2.66
_cell_volume                     4903.86(15)
_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 0.988
_diffrn_measurement_details
;
 3802 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Basel-Cu-Stoe
_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  0.0419
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            97842
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.152
_diffrn_reflns_theta_min         2.659
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.113
_exptl_absorpt_correction_T_max  0.4534
_exptl_absorpt_correction_T_min  0.3126
_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    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.180
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00259(12)
_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   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         9704
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0829
_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^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8338
_reflns_number_total             9704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00355h2.cif
_cod_data_source_block           scd011_150k
_cod_depositor_comments
'Adding full bibliography for 7246701--7246704.cif.'
_cod_database_code               7246704
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.631
_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. Uiso/Uaniso restraints and constraints
C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C15(H15A,H15B), C12(H12A,H12B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C26(H26), C30(H30), C28(H28), C27(H27), C35(H35), C20(H20),
 C34(H34), C53(H53), C57(H57), C24(H24), C41(H41), C47(H47), C29(H29), C56(H56),
  C2(H2), C43(H43), C4(H4), C9(H9), C55(H55), C7(H7), C42(H42), C23(H23),
 C3(H3), C54(H54), C8(H8), C21(H21), C22(H22), C51(H51), C48(H48), C49(H49),
 C50(H50)
4.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C44(H44A,H44B,H44C)
4.d :
 C18(H18), C14(H14)
;
_shelx_res_checksum              86755
_olex2_date_sample_data_collection 2022-10-07
_olex2_date_sample_submission    2022-10-03
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id SCD011_150K
_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 98.8
_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 146.4
_stoe_evaluation_lana_max_2theta_desired 146.4
_stoe_evaluation_lana_mean_redundancy 10.1
_stoe_evaluation_lana_number_refls_after_or 97872
_stoe_evaluation_lana_number_refls_outliers 26097
_stoe_evaluation_lana_number_refls_total 123969
_stoe_evaluation_lana_number_refls_unique 9711
_stoe_evaluation_lana_number_refls_written 97872
_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          12.6   28.4   44.2   60.0   75.8   91.6  107.4  123.2  139.0
<Resolution>    5.70   2.94   2.03   1.50   1.25   1.08   0.95   0.88   0.83
N(total)         198   2118   5013  13270  26403  27901  18538  20124  10404
<Redundancy>     2.4    5.3    5.8   10.2   15.4   13.9    8.1    9.3    6.5
Complet. [%%]    95.2  100.0  100.0  100.0  100.0  100.0  100.0  100.1   91.8
<I/sigma>      169.5   87.2   52.9   26.4   17.4   13.0    9.2    5.8    3.4
R(int)         0.017  0.024  0.023  0.032  0.037  0.042  0.075  0.188  0.298
;
_stoe_measurement_identifier     SCD011_150K
_stoe_measurement_max_exposure_per_frame '10.0 s'
_stoe_measurement_mean_exposure_per_frame '9.7 s'
_stoe_measurement_min_exposure_per_frame '2.5 s'
_stoe_measurement_total_exposure_time '10.2 h'
_stoe_measurement_total_frame_number 3802
_stoe_measurement_total_run_number 35
_stoe_measurement_tube_power     '50.0 W'