Controlling Molecular Organization by Using Phenyl Embraces of Multiple Trityl Groups.
Duong, Adam; Levesque, Alexandre; Homand, Clara; Maris, Thierry; Wuest, James D.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b02974

data_4038009
_publ_section_title
;
 Controlling Molecular Organization by Using Phenyl Embraces of Multiple
 Trityl Groups.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02974
_journal_year                    2020
_chemical_formula_moiety         'C188 H132 N4 Pd, 2(B F4)'
_chemical_formula_sum            'C188 H132 B2 F8 N4 Pd'
_chemical_formula_weight         2726.99
_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
_audit_creation_date             2015-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                108.741(2)
_cell_angle_beta                 106.946(2)
_cell_angle_gamma                99.339(2)
_cell_formula_units_Z            1
_cell_length_a                   13.0587(6)
_cell_length_b                   15.6881(8)
_cell_length_c                   21.3941(9)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    150
_cell_measurement_theta_max      62.563
_cell_measurement_theta_min      3.072
_cell_volume                     3808.6(3)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2004)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53044
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         76.300
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'Bruker Microstar Rotating Anode Generator'
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0807 before and 0.0666 after correction.
The Ratio of minimum to maximum transmission is 0.8337.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
Attempts to  model disordered solvent molecules
were unsuccessful. PLATON/SQUEEZE  was used to correct
the data for the presence of the disordered solvent.
A potential solvent volume of 440.9 \%A^3^, 
11.6 % of the total unit-cell volume, was found.
90 electrons per unit cell worth of scattering were located
in the void. The reported structure is based on the 
PLATON/SQUEEZE corrected data. The actual solvent content is
unknown, so several quantities calculated like empirical formula, density, 
absorption coefficient, F(000) etc. may be incorrect.

Ref:  Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201.
;
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         13526
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1042P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10914
_reflns_number_total             13526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02974_si_008.cif
_cod_data_source_block           adam10
_cod_database_code               4038009
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C28-C29
 1.53 with sigma of 0.001
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48,
 C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64,
  C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79,
 C80, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92, C93, C94, N1,
 N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C50(H50), C52(H52), C57(H57), C58(H58),
 C59(H59), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67),
  C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C78(H78), C79(H79),
 C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88),
  C90(H90), C91(H91), C92(H92), C93(H93), C94(H94)
4.b Fitted hexagon refined as free rotating group:
 C9(C10,C11,C12,C13,C14), C15(C16,C17,C18,C19,C20), C21(C22,C23,C24,C25,C26),
 C30(C31,C32,C33,C34,C35), C36(C37,C38,C39,C40,C41), C42(C43,C44,C45,C46,C47),
 C56(C57,C58,C59,C60,C61), C62(C63,C64,C65,C66,C67), C68(C69,C70,C71,C72,C73),
 C77(C78,C79,C80,C81,C82), C83(C84,C85,C86,C87,C88), C89(C90,C91,C92,C93,C94)
;
_shelx_res_checksum              64058
_shelx_hkl_checksum              53668
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'