Structural Data Showing the Existence of LDI Bonds between the Rings of Dimeric Cofacial Siloxysilicon Phthalocyanines.
Sturtz, Benjamin W.; Moore, Curtis E.; Jenkins, Tyler S.; Miller, Jennifer L.; Momberger, Carlisle D.; Rheingold, Arnold L.; Kenney, Malcolm E.; The journal of physical chemistry. A 123 (2019) 471–481; doi:10.1021/acs.jpca.8b09247

data_1552808
_publ_section_title
;
 Structural Data Showing the Existence of LDI Bonds between the Rings of
 Dimeric Cofacial Siloxysilicon Phthalocyanines.
;
_journal_issue                   2
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              471
_journal_page_last               481
_journal_paper_doi               10.1021/acs.jpca.8b09247
_journal_volume                  123
_journal_year                    2019
_chemical_formula_moiety         'C82 H74 N16 O3 Si4'
_chemical_formula_sum            'C82 H74 N16 O3 Si4'
_chemical_formula_weight         1443.93
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.104(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.076(3)
_cell_length_b                   23.344(6)
_cell_length_c                   23.162(5)
_cell_measurement_reflns_used    7548
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.34
_cell_volume                     7070(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37854
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.745
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  0.2645
_exptl_absorpt_correction_T_min  0.2004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0691 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.7577.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.804
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         12316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+8.3766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8886
_reflns_number_total             12316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp8b09247_si_004.cif
_cod_data_source_block           kenney23_a
_cod_database_code               1552808
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.951
_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:
 C65(H65A,H65B), C66(H66A,H66B), C68(H68A,H68B), C69(H69A,H69B), C71(H71A,
 H71B), C72(H72A,H72B), C74(H74A,H74B), C75(H75A,H75B), C77(H77A,H77B),
 C78(H78A,H78B), C80(H80A,H80B), C81(H81A,H81B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C18(H18), C19(H19), C20(H20), C21(H21), C26(H26), C27(H27), C28(H28), C29(H29),
  C33(H33), C34(H34), C35(H35), C36(H36), C41(H41), C42(H42), C43(H43),
 C44(H44), C49(H49), C50(H50), C51(H51), C52(H52), C57(H57), C58(H58), C59(H59),
  C60(H60)
2.c Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C76(H76A,H76B,
 H76C), C79(H79A,H79B,H79C), C82(H82A,H82B,H82C)
;
_shelx_res_checksum              35933
_shelx_hkl_checksum              2437
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'