The effects of introducing terminal alkenyl substituents into the 2,2'-bipyridine domain in [Cu(N^N)(P^P)]+ coordination compounds
Wöhler, Jannika; Meyer, Marco; Prescimone, Alessandro; Constable, Edwin C.; Housecroft, Catherine E.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01799G

data_7710952
_publ_section_title
;
 The effects of introducing terminal alkenyl substituents into the
 2,2'-bipyridine domain in [Cu(N^N)(P^P)]+ coordination compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01799G
_journal_year                    2022
_chemical_formula_moiety         'C54 H48 Cu N2 O P2, F6 P, 1[CH2Cl2]'
_chemical_formula_sum            'C55 H50 Cl2 Cu F6 N2 O P3'
_chemical_formula_weight         1096.32
_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             2021-08-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-05-06 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                104.521(3)
_cell_angle_beta                 98.067(4)
_cell_angle_gamma                110.792(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9227(5)
_cell_length_b                   13.4650(6)
_cell_length_c                   18.5972(8)
_cell_measurement_reflns_used    78381
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.61
_cell_measurement_theta_min      2.54
_cell_volume                     2613.8(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.969
_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  0.0691
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40293
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.389
_diffrn_reflns_theta_min         2.537
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.923
_exptl_absorpt_correction_T_max  0.2058
_exptl_absorpt_correction_T_min  0.0710
_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    1.393
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         9708
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1428P)^2^+1.9527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8577
_reflns_number_total             9708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01799g2.cif
_cod_data_source_block           woj057_150k
_cod_database_code               7710952
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.529
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C58-C15 \\sim C14-C13 \\sim C21-C19 \\sim C20-C19
 with sigma of 0.02
 C21-C19 \\sim C20-C19 \\sim C14-C13 \\sim C58-C15
 with sigma of 0.005
3. Others
 Fixed Sof: H11A(0.5) H11B(0.5) H11C(0.5) H11D(0.5) H19A(0.5) H19(0.5)
 C12(0.5) H12A(0.5) H12B(0.5) C20(0.5) H20A(0.5) H20B(0.5) C21(0.5) H21A(0.5)
 H21B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C14(0.5) H14A(0.5) H14B(0.5) C15(0.5)
 H15(0.5) C13(0.5) H13(0.5) C58(0.5) H58A(0.5) H58B(0.5)
4.a Riding coordinates:
 C58(H58A,H58B)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C11(H11C,H11D), C17(H17A,H17B), C18(H18A,H18B), C12(H12A,
 H12B), C16(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C42(H42), C53(H53), C44(H44), C39(H39), C47(H47), C51(H51),
 C48(H48), C36(H36), C43(H43), C38(H38), C23(H23), C49(H49), C7(H7), C27(H27),
 C37(H37), C50(H50), C54(H54), C26(H26), C9(H9), C8(H8), C57(H57), C29(H29),
 C33(H33), C31(H31), C30(H30), C24(H24), C4(H4), C55(H55), C2(H2), C25(H25),
 C32(H32), C3(H3), C56(H56), C19(H19A), C19(H19), C15(H15), C13(H13)
4.d X=CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C14(H14A,H14B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30219
_shelx_fab_checksum              48382
_olex2_date_sample_data_collection 2021-08-17
_olex2_date_sample_submission    2021-07-18
_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 WOJ057_150K
_olex2_submission_special_instructions 'No special instructions were received'