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_4038006
_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         'C104 H76 N4 Pd, 2(B F4), 2(C6 H14)'
_chemical_formula_sum            'C116 H104 B2 F8 N4 Pd'
_chemical_formula_weight         1834.05
_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
_audit_creation_date             2015-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                106.603(4)
_cell_angle_beta                 96.033(4)
_cell_angle_gamma                100.512(4)
_cell_formula_units_Z            2
_cell_length_a                   9.1474(11)
_cell_length_b                   21.215(2)
_cell_length_c                   26.637(3)
_cell_measurement_reflns_used    3319
_cell_measurement_temperature    150
_cell_measurement_theta_max      43.123
_cell_measurement_theta_min      2.229
_cell_volume                     4802.3(9)
_computing_cell_refinement       'SAINT v7.46A (Bruker, 2008)'
_computing_data_collection       'APEX2 v2.1-0 (Bruker AXS, 2006a)'
_computing_data_reduction        'SAINT v7.46A (Bruker, 2008)'
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.712
_diffrn_measured_fraction_theta_max 0.712
_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  0.084
_diffrn_reflns_av_unetI/netI     0.2822
_diffrn_reflns_Laue_measured_fraction_full 0.712
_diffrn_reflns_Laue_measured_fraction_max 0.712
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            74792
_diffrn_reflns_point_group_measured_fraction_full 0.712
_diffrn_reflns_point_group_measured_fraction_max 0.712
_diffrn_reflns_theta_full        67.511
_diffrn_reflns_theta_max         67.511
_diffrn_reflns_theta_min         1.755
_exptl_absorpt_coefficient_mu    2.101
_exptl_absorpt_correction_T_max  0.8059
_exptl_absorpt_correction_T_min  0.6521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/4 (Bruker,2007/4) was used for absorption correction.
wR2(int) was 0.1109 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.8092.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1148
_refine_ls_number_reflns         12317
_refine_ls_number_restraints     355
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0089P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3918
_reflns_number_total             12317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02974_si_005.cif
_cod_data_source_block           jw1336
_cod_original_cell_volume        4802.4(10)
_cod_database_code               4038006
_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
 C200-C201 = C201-C202 = C202-C203 = C203-C204 = C204-C205
 1.53 with sigma of 0.001
 C200-C202 = C201-C203 = C202-C204 = C203-C205
 2.35 with sigma of 0.001
 C200-C205
 3.2 with sigma of 0.001
 C300-C301 = C301-C302 = C302-C303 = C303-C304 = C304-C305
 1.53 with sigma of 0.001
 C300-C302 = C301-C303 = C302-C304 = C303-C305
 2.35 with sigma of 0.001
 C210-C211 = C211-C212 = C212-C213 = C213-C214 = C214-C215
 1.53 with sigma of 0.001
 C210-C212 = C211-C213 = C212-C214 = C213-C215
 2.35 with sigma of 0.001
 C310-C311 = C311-C312 = C312-C313 = C313-C314 = C314-C315
 1.53 with sigma of 0.001
 C310-C312 = C311-C313 = C312-C314 = C313-C315
 2.35 with sigma of 0.001
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: C200(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C201(0.5) H20D(0.5)
 H20E(0.5) C202(0.5) H20F(0.5) H20G(0.5) C203(0.5) H20H(0.5) H20I(0.5)
 C204(0.5) H20J(0.5) H20K(0.5) C205(0.5) H20L(0.5) H20M(0.5) H20N(0.5)
 C300(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C301(0.5) H30D(0.5) H30E(0.5)
 C302(0.5) H30F(0.5) H30G(0.5) C303(0.5) H30H(0.5) H30I(0.5) C304(0.5)
 H30J(0.5) H30K(0.5) C305(0.5) H30L(0.5) H30M(0.5) H30N(0.5) C210(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) C211(0.5) H21D(0.5) H21E(0.5) C212(0.5)
 H21F(0.5) H21G(0.5) C213(0.5) H21H(0.5) H21I(0.5) C214(0.5) H21J(0.5)
 H21K(0.5) C215(0.5) H21L(0.5) H21M(0.5) H21N(0.5) C310(0.5) H31A(0.5)
 H31B(0.5) H31C(0.5) C311(0.5) H31D(0.5) H31E(0.5) C312(0.5) H31F(0.5)
 H31G(0.5) C313(0.5) H31H(0.5) H31I(0.5) C314(0.5) H31J(0.5) H31K(0.5)
 C315(0.5) H31L(0.5) H31M(0.5) H31N(0.5)
 Fixed Uiso: C200(0.15) C201(0.15) C202(0.15) C203(0.15) C204(0.15) C205(0.15)
 C300(0.15) C301(0.15) C302(0.15) C303(0.15) C304(0.15) C305(0.15) C210(0.15)
 C211(0.15) C212(0.15) C213(0.15) C214(0.15) C215(0.15) C310(0.15) C311(0.15)
 C312(0.15) C313(0.15) C314(0.15) C315(0.15)
5.a Secondary CH2 refined with riding coordinates:
 C201(H20D,H20E), C202(H20F,H20G), C203(H20H,H20I), C204(H20J,H20K), C301(H30D,
 H30E), C302(H30F,H30G), C303(H30H,H30I), C304(H30J,H30K), C211(H21D,H21E),
 C212(H21F,H21G), C213(H21H,H21I), C214(H21J,H21K), C311(H31D,H31E), C312(H31F,
 H31G), C313(H31H,H31I), C314(H31J,H31K)
5.b Me refined with riding coordinates:
 C210(H21A,H21B,H21C), C215(H21L,H21M,H21N), C310(H31A,H31B,H31C), C315(H31L,
 H31M,H31N)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), 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), C27(H27), C28(H28), C30(H30), C31(H31),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C56(H56), C57(H57), C62(H62), C63(H63), C64(H64), C65(H65),
  C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74),
 C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83),
  C88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C94(H94), C95(H95),
 C96(H96), C97(H97), C98(H98), C100(H100), C101(H101), C102(H102), C103(H103),
 C104(H104)
5.d Idealised Me refined as rotating group:
 C200(H20A,H20B,H20C), C205(H20L,H20M,H20N), C300(H30A,H30B,H30C), C305(H30L,
 H30M,H30N)
;
_shelx_res_checksum              9981
_shelx_hkl_checksum              31744
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'