IPr# - Highly Hindered, Broadly Applicable N-Heterocyclic Carbenes
Zhao, Qun; Meng, Guangrong; Li, Guangchen; Flach, Carol R.; Mendelsohn, Richard; Lalancette, Roger A.; Szostak, Roman; Szostak, Michal; Chemical Science  (2021) –; doi:10.1039/D1SC02619D

data_1563905
_publ_section_title
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 IPr# - Highly Hindered, Broadly Applicable N-Heterocyclic Carbenes
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02619D
_journal_year                    2021
_chemical_formula_moiety         'C102 H81 Cl N2 Pd, 2(C H2 Cl2)'
_chemical_formula_sum            'C104 H85 Cl5 N2 Pd'
_chemical_formula_weight         1646.40
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
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2021-04-12 deposited with the CCDC.	2021-06-29 downloaded from the CCDC.
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_cell_angle_alpha                99.161(4)
_cell_angle_beta                 95.616(5)
_cell_angle_gamma                102.560(4)
_cell_formula_units_Z            2
_cell_length_a                   14.037(1)
_cell_length_b                   15.0707(11)
_cell_length_c                   21.0521(15)
_cell_measurement_reflns_used    9031
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.00
_cell_measurement_theta_min      3.06
_cell_volume                     4250.7(5)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'Bruker SMART CCD Apex-II area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.899
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35885
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.730
_diffrn_reflns_theta_min         2.146
_exptl_absorpt_coefficient_mu    3.583
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.138
_platon_squeeze_details
;
SQUEEZE calculated 70 electrons per cell, which is attributed to 
one disordered DCM molecule and one methanol and one water of 
crystallization.
;
_refine_diff_density_max         1.485
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         13860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0855P)^2^+13.7136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11572
_reflns_number_total             13860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02619d2.cif
_cod_data_source_block           MENG_ROGER_a_sq
_cod_original_cell_volume        4250.6(5)
_cod_database_code               1563905
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.273
_shelx_estimated_absorpt_t_max   0.638
_shelx_res_checksum              13351
_shelx_hkl_checksum              37834