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_7710950
_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         'C57 H56 Cu N2 O P2, F6 P'
_chemical_formula_sum            'C57 H56 Cu F6 N2 O P3'
_chemical_formula_weight         1055.48
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-03
_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                90
_cell_angle_beta                 110.268(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4311(3)
_cell_length_b                   15.1404(3)
_cell_length_c                   20.4627(4)
_cell_measurement_reflns_used    97538
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.75
_cell_measurement_theta_min      3.72
_cell_volume                     5066.01(18)
_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 0.993
_diffrn_measured_fraction_theta_max 0.975
_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  0.0196
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43735
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.373
_diffrn_reflns_theta_min         3.718
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.046
_exptl_absorpt_correction_T_max  0.2373
_exptl_absorpt_correction_T_min  0.1828
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00154(10)
_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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         9442
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0780P)^2^+5.6157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9355
_reflns_number_total             9442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01799g2.cif
_cod_data_source_block           woj056_150k
_cod_database_code               7710950
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.629
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-C13
 1.52 with sigma of 0.005
 C16-C15 \\sim C19-C15 \\sim C17-C16 \\sim C20-C19 \\sim C20-C21 \\sim C18-C17
 with sigma of 0.02
 C21-C20 \\sim C18-C17 \\sim C17-C16 \\sim C20-C19 \\sim C16-C15 \\sim C19-C15
\\sim C14-C13 \\sim C13-C12
 \\sim C12-C11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16) = Uanis(C17) = Uanis(C21) = Uanis(C19) = Uanis(C20) = Uanis(C18)
4. Others
 Fixed Sof: H15A(0.7) H15B(0.7) H15C(0.3) H15D(0.3) C16(0.7) H16A(0.7)
 H16B(0.7) C17(0.7) H17A(0.7) H17B(0.7) C21(0.3) H21A(0.3) H21B(0.3) H21C(0.3)
 C19(0.3) H19A(0.3) H19B(0.3) C20(0.3) H20A(0.3) H20B(0.3) C18(0.7) H18A(0.7)
 H18B(0.7) H18C(0.7)
5.a Riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B,H14C)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C15(H15A,H15B), C15(H15C,H15D), C12(H12A,H12B), C16(H16A,
 H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C44(H44), C39(H39), C50(H50), C56(H56), C29(H29), C42(H42), C60(H60),
 C23(H23), C38(H38), C43(H43), C37(H37), C30(H30), C54(H54), C33(H33), C51(H51),
  C31(H31), C24(H24), C25(H25), C58(H58), C59(H59), C53(H53), C27(H27),
 C52(H52), C57(H57), C7(H7), C26(H26), C9(H9), C32(H32), C2(H2), C4(H4), C8(H8),
  C3(H3)
5.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C21(H21A,H21B,H21C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              26812
_olex2_date_sample_submission    2021-07-03
_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 WOJ056_150K
_olex2_submission_special_instructions 'No special instructions were received'