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_7710951
_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, F5.25 P, 0.75(F)'
_chemical_formula_sum            'C54 H48 Cu F6 N2 O P3'
_chemical_formula_weight         1011.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-06 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9358(2)
_cell_length_b                   20.1224(2)
_cell_length_c                   21.6456(4)
_cell_measurement_reflns_used    86834
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.99
_cell_measurement_theta_min      4.10
_cell_volume                     4740.94(13)
_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 1.5 (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 0.995
_diffrn_measured_fraction_theta_max 0.980
_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  0.0201
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48448
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.678
_diffrn_reflns_theta_min         4.104
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.163
_exptl_absorpt_correction_T_max  0.4385
_exptl_absorpt_correction_T_min  0.3583
_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    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         9239
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0670P)^2^+4.7922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8304
_reflns_number_total             9239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01799g2.cif
_cod_data_source_block           woj093_150k
_cod_database_code               7710951
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.603
_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
 P3-F3 = P3-F2
 1.6 with sigma of 0.001
 P3-F10 = P3-F11
 1.6 with sigma of 0.001
 F10-P3 = P3-F9
 1.6 with sigma of 0.001
 F6-P3 = P3-F9
 1.6 with sigma of 0.001
 P3-F6 = P3-F9
 1.6 with sigma of 0.001
 P3-F8 = P3-F2
 1.6 with sigma of 0.001
 P3-F11 = P3-F2
 1.6 with sigma of 0.001
 F12-F8 \\sim F12-F6 \\sim F8-F10 \\sim F6-F10
 with sigma of 0.04
 P3-F12 \\sim P3-F8 \\sim P3-F6 \\sim P3-F4 \\sim P3-F10 \\sim P3-F1
 with sigma of 0.02
 F7-F14 \\sim F7-F9 \\sim F14-F2 \\sim F9-F2
 with sigma of 0.04
 P3-F7 \\sim P3-F14 \\sim P3-F4 \\sim P3-F1 \\sim P3-F9 \\sim P3-F2
 with sigma of 0.02
 P3-F13 \\sim P3-F5 \\sim P3-F4 \\sim P3-F1 \\sim P3-F3 \\sim P3-F11
 with sigma of 0.02
 F13-F5 \\sim F13-F3 \\sim F5-F11 \\sim F3-F11
 with sigma of 0.04
3. Others
 Fixed Sof: F6(0.5) F8(0.5) F10(0.5) F12(0.5) F14(0.25) F7(0.25) F2(0.25)
 F9(0.25) F5(0.25) F11(0.25) F3(0.25) F13(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C19(H19), C21(H21), C28(H28), C38(H38), C32(H32),
 C20(H20), C41(H41), C42(H42), C50(H50), C44(H44), C48(H48), C40(H40), C51(H51),
  C39(H39), C54(H54), C45(H45), C46(H46), C47(H47), C52(H52), C35(H35),
 C33(H33), C36(H36), C2(H2), C53(H53), C4(H4), C34(H34), C9(H9), C3(H3),
 C14(H14), C7(H7), C8(H8)
4.c X=CH2 refined with riding coordinates:
 C15(H15A,H15B)
4.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              5736
_olex2_date_sample_data_collection 2021-12-09
_olex2_date_sample_submission    2021-12-04
_olex2_exptl_crystal_mounting_method
;
The crystal was mounted on a mylar loop in perfluoroether oil
;
_olex2_submission_original_sample_id WOJ093
_olex2_submission_special_instructions 'No special instructions were received'