Chelated bis(NHC) complexes of saturated (imidazolin-2-ylidene) NHC ligands: structural authentication and facile ligand fragmentation.
Gardiner, Michael G.; McGuinness, David S.; Vanston, Catriona R.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3051–3058; doi:10.1039/c7dt00327g

data_7042019
_publ_section_title
;
 Chelated bis(NHC) complexes of saturated (imidazolin-2-ylidene) NHC
 ligands: structural authentication and facile ligand fragmentation.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3051
_journal_page_last               3058
_journal_paper_doi               10.1039/c7dt00327g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C29 H38 N6 Pd, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C31 H41 F12 N7 P2 Pd'
_chemical_formula_weight         908.05
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-15 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.25(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.136(2)
_cell_length_b                   6.839(1)
_cell_length_c                   24.481(3)
_cell_measurement_reflns_used    30991
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      1.52
_cell_volume                     3712.8(18)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            40557
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         1.52
_diffrn_source                   'Synchrotron BM'
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.760
_refine_diff_density_min         -3.142
_refine_diff_density_rms         0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.1173
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1255P)^2^+80.4366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3132
_refine_ls_wR_factor_ref         0.3158
_reflns_number_gt                9911
_reflns_number_total             10748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00327g1.cif
_cod_data_source_block           79cv93a
_cod_depositor_comments
'Adding full bibliography for 7042016--7042022.cif.'
_cod_original_cell_volume        3712.8(13)
_cod_database_code               7042019
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C19(H19), C21(H21)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C), C31(H31A,H31B,H31C)
;
_olex2_submission_original_sample_id as79cv93a
_olex2_submission_special_instructions 'No special instructions were received'