Heteroleptic [Cu(P^P)(N^N)][PF6] Complexes: Effects of Isomer Switching from 2,2′-biquinoline to 1,1′-biisoquinoline
Arnosti, Nina; Meyer, Marco; Prescimone, Alessandro; Constable, Edwin; Housecroft, Catherine; Crystals 11 (2021) 185–; doi:10.3390/cryst11020185

data_1566038
_publ_section_title
;
 Heteroleptic [Cu(P^P)(N^N)][PF6] Complexes: Effects of Isomer Switching
 from 2,2&#x2032;-biquinoline to 1,1&#x2032;-biisoquinoline
;
_journal_issue                   2
_journal_name_full               Crystals
_journal_page_first              185
_journal_paper_doi               10.3390/cryst11020185
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C54 H40 Cu N2 O P2, F6 P, 0.5(C4 H10 O)'
_chemical_formula_sum            'C56 H45 Cu F6 N2 O1.5 P3'
_chemical_formula_weight         1040.39
_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
_cell_angle_alpha                92.018(2)
_cell_angle_beta                 91.054(2)
_cell_angle_gamma                112.546(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4728(3)
_cell_length_b                   14.2115(4)
_cell_length_c                   16.0992(4)
_cell_measurement_reflns_used    88836
_cell_measurement_temperature    150
_cell_measurement_theta_max      58.67
_cell_measurement_theta_min      2.39
_cell_volume                     2421.34(12)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
X-Area X-Red32 1.65.0.0 (STOE, 2018)
;
_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 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_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  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33930
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         58.164
_diffrn_reflns_theta_min         2.391
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    3.409
_exptl_absorpt_correction_T_max  0.5170
_exptl_absorpt_correction_T_min  0.4058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0013(2)
_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   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         10023
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0847P)^2^+0.9980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9750
_reflns_number_total             10023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Crystals-2021-11-2-185.cif
_cod_data_source_block           arn039_150k
_cod_original_formula_sum        'C56 H45 Cu F6 N2 O1.50 P3'
_cod_database_code               1566038
_shelx_estimated_absorpt_t_max   0.579
_shelx_estimated_absorpt_t_min   0.508
_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-C57
 1.41 with sigma of 0.02
 O2-C55
 1.42 with sigma of 0.02
 C58-C57
 1.48 with sigma of 0.02
 C55-C56
 1.5 with sigma of 0.02
 O2-C58 = O2-C56
 2.37 with sigma of 0.04
 C58-O2 \\sim O2-C56
 with sigma of 0.04
 O2-C57 \\sim O2-C55
 with sigma of 0.02
 C58-C57 \\sim C55-C56
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C58 \\sim C57 \\sim C55 \\sim C56: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O2, C58, C57, C55, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O2(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C57(0.5) H57A(0.5)
 H57B(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5)
6.a Riding coordinates:
 C58(H58A,H58B,H58C), C57(H57A,H57B), C55(H55A,H55B), C56(H56A,H56B,H56C)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C32(H32), C40(H40), C30(H30), C11(H11), C27(H27), C42(H42), C2(H2),
 C29(H29), C41(H41), C50(H50), C39(H39), C9(H9), C14(H14), C20(H20), C16(H16),
 C54(H54), C51(H51), C1(H1), C36(H36), C44(H44), C15(H15), C10(H10), C33(H33),
 C28(H28), C13(H13), C35(H35), C24(H24), C17(H17), C34(H34), C48(H48), C45(H45),
  C18(H18), C21(H21), C53(H53), C52(H52), C47(H47), C22(H22), C46(H46), C23(H23)
;
_shelx_res_checksum              70870
_shelx_hkl_checksum              12703
_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 ARN039
_olex2_submission_special_instructions 'No special instructions were received'