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_7246701
_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         'C54 H44 Cu N2 O P2, F6 P'
_chemical_formula_sum            'C54 H44 Cu F6 N2 O P3'
_chemical_formula_weight         1007.36
_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             2022-11-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-28 deposited with the CCDC.	2023-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.5070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8682(2)
_cell_length_b                   32.7516(8)
_cell_length_c                   13.6339(2)
_cell_measurement_reflns_used    67165
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.00
_cell_measurement_theta_min      2.70
_cell_volume                     4799.61(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
 2318 frames, detector distance = 40 mm
;
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            56154
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.113
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.136
_exptl_absorpt_correction_T_max  0.4564
_exptl_absorpt_correction_T_min  0.3032
_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    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.180
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.00137(7)
_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   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0871
_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^)+(0.0300P)^2^+24.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.1900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8033
_reflns_number_total             9442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00355h2.cif
_cod_data_source_block           scd010_150k
_cod_depositor_comments
'Adding full bibliography for 7246701--7246704.cif.'
_cod_database_code               7246701
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.784
_shelx_estimated_absorpt_t_min   0.651
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C47(H47A,H47B), C52(H52A,H52B), C48(H48A,H48B)
2.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C36(H36), C21(H21), C22(H22), C23(H23), C24(H24), C33(H33),
 C35(H35), C15(H15), C18(H18), C26(H26), C34(H34), C2(H2), C29(H29), C30(H30),
 C17(H17), C28(H28), C16(H16), C40(H40), C27(H27), C3(H3), C8(H8), C45(H45),
 C4(H4), C6(H6), C12(H12), C38(H38), C43(H43), C39(H39), C5(H5), C44(H44),
 C9(H9), C11(H11), C10(H10)
2.c :
 C50(H50), C54(H54)
;
_shelx_res_checksum              30305
_olex2_date_sample_data_collection 2022-11-17
_olex2_date_sample_submission    2022-10-18
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id SCD010
_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 98.3
_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 146.3
_stoe_evaluation_lana_max_2theta_desired 146.3
_stoe_evaluation_lana_mean_redundancy 5.9
_stoe_evaluation_lana_number_refls_after_or 56159
_stoe_evaluation_lana_number_refls_outliers 18708
_stoe_evaluation_lana_number_refls_total 74867
_stoe_evaluation_lana_number_refls_unique 9445
_stoe_evaluation_lana_number_refls_written 56159
_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          14.0   29.6   45.2   60.8   76.4   92.0  107.6  123.2  138.8
<Resolution>    5.21   2.86   1.98   1.48   1.25   1.07   0.95   0.88   0.83
N(total)         159   1259   2930   8184  15434  16413  11580  12460   6448
<Redundancy>     1.9    3.0    3.4    6.1    8.6    7.8    5.1    5.7    4.1
Complet. [%%]    96.0  100.0  100.0  100.0  100.0  100.0   99.7   99.3   89.1
<I/sigma>      220.2  101.0   58.8   31.4   21.1   16.3   11.0    7.0    3.8
R(int)         0.020  0.032  0.028  0.038  0.036  0.040  0.072  0.178  0.274
;
_stoe_measurement_identifier     SCD010_150K
_stoe_measurement_max_exposure_per_frame '5.0 s'
_stoe_measurement_mean_exposure_per_frame '4.9 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '3.1 h'
_stoe_measurement_total_frame_number 2318
_stoe_measurement_total_run_number 22
_stoe_measurement_tube_power     '50.0 W'