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_1552811
_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         'C88 H86 N16 O3 Si4'
_chemical_formula_sum            'C88 H86 N16 O3 Si4'
_chemical_formula_weight         1528.08
_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     dual
_audit_creation_date             2017-06-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                77.793(3)
_cell_angle_beta                 81.704(3)
_cell_angle_gamma                76.746(3)
_cell_formula_units_Z            4
_cell_length_a                   13.7795(13)
_cell_length_b                   22.430(2)
_cell_length_c                   26.079(2)
_cell_measurement_reflns_used    9565
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.139
_cell_measurement_theta_min      2.325
_cell_volume                     7629.3(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            170662
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.124
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0930 before and 0.0573 after correction. The Ratio of minimum to maximum transmission is 0.8784. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       plate
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2132
_refine_ls_number_reflns         26869
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0612P)^2^+15.5475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18519
_reflns_number_total             26869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp8b09247_si_002.cif
_cod_data_source_block           kenney56_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        7629.0(13)
_cod_database_code               1552811
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.964
_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
 Si08-C173 = Si08-C176 = Si08-C185
 1.87 with sigma of 0.005
 C185-C186 = C187-C186 = C187-C189 = C176-C182 = C178-C182 = C179-C178 = C173-
 C172 = C171-C172 = C171-C170
 1.54 with sigma of 0.005
 Si8-C166 = Si8-C174 = Si8-C183
 1.87 with sigma of 0.005
 C167-C166 = C167-C168 = C168-C169 = C175-C174 = C175-C181 = C181-C180 = C183-
 C184 = C184-C188 = C190-C188
 1.54 with sigma of 0.005
 C176-C178
 2.54 with sigma of 0.01
 C173-C171
 2.54 with sigma of 0.01
 C185-C187
 2.54 with sigma of 0.01
 C182-C179
 2.54 with sigma of 0.01
 C172-C170
 2.54 with sigma of 0.01
 C186-C189
 2.54 with sigma of 0.01
 C166-C168
 2.54 with sigma of 0.01
 C174-C181
 2.54 with sigma of 0.01
 C183-C188
 2.54 with sigma of 0.01
 C167-C169
 2.54 with sigma of 0.01
 C175-C180
 2.54 with sigma of 0.01
 C184-C190
 2.54 with sigma of 0.01
3. Rigid body (RIGU) restrains
 Si08, C185, C186, C187, C173, C172, C171, C170, C176, C182, C189, C178, C179,
 O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O6, Si8, C183, C184, C188, C190, C166, C167, C168, C169, C174, C175, C181, C180
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C169)=Sof(H16O)=Sof(H16P)=Sof(H16Q)=Sof(C168)=Sof(H16R)=Sof(H16S)=
 Sof(C167)=Sof(H16T)=Sof(H16U)=Sof(C166)=Sof(H16V)=Sof(H16W)=Sof(Si8)=Sof(C174)=
 Sof(H17Q)=Sof(H17R)=Sof(C175)=Sof(H17S)=Sof(H17T)=Sof(C181)=Sof(H18L)=
 Sof(H18M)=Sof(C180)=Sof(H18N)=Sof(H18O)=Sof(H18P)=Sof(C183)=Sof(H18Q)=
 Sof(H18R)=Sof(C184)=Sof(H18S)=Sof(H18T)=Sof(C188)=Sof(H18U)=Sof(H18V)=
 Sof(C190)=Sof(H19A)=Sof(H19B)=Sof(H19C)=1-FVAR(1)
 Sof(Si08)=Sof(C172)=Sof(H17A)=Sof(H17B)=Sof(C171)=Sof(H17C)=Sof(H17D)=
 Sof(C189)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C182)=Sof(H18D)=Sof(H18E)=
 Sof(C170)=Sof(H17E)=Sof(H17F)=Sof(H17G)=Sof(C186)=Sof(H18F)=Sof(H18G)=
 Sof(C185)=Sof(H18H)=Sof(H18I)=Sof(C178)=Sof(H17H)=Sof(H17I)=Sof(C173)=
 Sof(H17J)=Sof(H17K)=Sof(C187)=Sof(H18J)=Sof(H18K)=Sof(C179)=Sof(H17L)=
 Sof(H17M)=Sof(H17N)=Sof(C176)=Sof(H17O)=Sof(H17P)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C158(H15A,H15B), C154(H15C,H15D), C162(H16A,H16B), C163(H16C,H16D), C155(H15E,
 H15F), C160(H16E,H16F), C172(H17A,H17B), C171(H17C,H17D), C182(H18D,H18E),
 C159(H15J,H15K), C164(H16M,H16N), C156(H15L,H15M), C186(H18F,H18G), C185(H18H,
 H18I), C178(H17H,H17I), C173(H17J,H17K), C187(H18J,H18K), C78(H78A,H78B),
 C81(H81A,H81B), C69(H69A,H69B), C86(H86A,H86B), C74(H74A,H74B), C05J(H05Z,H),
 C79(H79A,H79B), C65(H65A,H65B), C87(H87A,H87B), C70(H70A,H70B), C71(H71A,H71B),
  C67(H67A,H67B), C75(H75A,H75B), C66(H66A,H66B), C82(H82A,H82B), C85(H85A,
 H85B), C77(H77A,H77B), C83(H83A,H83B), C176(H17O,H17P), C168(H16R,H16S),
 C167(H16T,H16U), C166(H16V,H16W), C174(H17Q,H17R), C175(H17S,H17T), C181(H18L,
 H18M), C183(H18Q,H18R), C184(H18S,H18T), C188(H18U,H18V)
5.b Aromatic/amide H refined with riding coordinates:
 C99(H99), C100(H100), C124(H124), C107(H107), C118(H118), C131(H131),
 C115(H115), C143(H143), C151(H151), C102(H102), C125(H125), C92(H92),
 C134(H134), C94(H94), C108(H108), C116(H116), C149(H149), C93(H93), C142(H142),
  C133(H133), C141(H141), C101(H101), C150(H150), C126(H126), C91(H91),
 C123(H123), C148(H148), C117(H117), C109(H109), C110(H110), C140(H140),
 C132(H132), C43(H43), C45(H45), C11(H11), C6(H6), C38(H38), C20(H20), C22(H22),
  C51(H51), C13(H13), C21(H21), C44(H44), C3(H3), C35(H35), C60(H60), C62(H62),
 C30(H30), C5(H5), C53(H53), C52(H52), C36(H36), C61(H61), C4(H4), C19(H19),
 C14(H14), C46(H46), C37(H37), C54(H54), C59(H59), C12(H12), C27(H27), C29(H29),
  C28(H28)
5.c Idealised Me refined as rotating group:
 C161(H16G,H16H,H16I), C157(H15G,H15H,H15I), C165(H16J,H16K,H16L), C189(H18A,
 H18B,H18C), C170(H17E,H17F,H17G), C179(H17L,H17M,H17N), C84(H84A,H84B,H84C),
 C68(H68A,H68B,H68C), C88(H88A,H88B,H88C), C76(H76A,H76B,H76C), C80(H80A,H80B,
 H80C), C72(H72A,H72B,H72C), C169(H16O,H16P,H16Q), C180(H18N,H18O,H18P),
 C190(H19A,H19B,H19C)
;
_shelx_res_checksum              13046
_shelx_hkl_checksum              9304
_olex2_submission_special_instructions 'No special instructions were received'