Synthesis of heteroatomic bridged paracyclophanes.
Reuter, K.; Maas, R. G. M.; Reuter, A.; Kilgenstein, F.; Asfaha, Y.; von Hänisch, C; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4530–4541; doi:10.1039/c7dt00321h

data_7042375
_publ_section_title
;
 Synthesis of heteroatomic bridged paracyclophanes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4530
_journal_page_last               4541
_journal_paper_doi               10.1039/c7dt00321h
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C18 H34 O2 Si2, 0.5(C H Cl3)'
_chemical_formula_sum            'C18.5 H34.5 Cl1.5 O2 Si2'
_chemical_formula_weight         398.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-01-13 deposited with the CCDC.
2017-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                104.231(2)
_cell_angle_beta                 105.552(2)
_cell_angle_gamma                101.563(2)
_cell_formula_units_Z            4
_cell_length_a                   12.4377(9)
_cell_length_b                   12.9833(8)
_cell_length_c                   15.6637(10)
_cell_measurement_reflns_used    7614
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.48
_cell_volume                     2263.9(3)
_computing_cell_refinement       'SAINT v8.34A (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    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0773
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41342
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.301
_diffrn_reflns_theta_max         25.301
_diffrn_reflns_theta_min         2.480
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1136 before and 0.0751 after correction.
The Ratio of minimum to maximum transmission is 0.9463.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_meas      1.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0349P)^2^+1.5976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6080
_reflns_number_total             8233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00321h1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
Adding full bibliography for 7042367--7042376.cif.

2017-11-20
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C18 H34 O2 Si2), C H Cl3'
_cod_original_formula_sum        'C37 H69 Cl3 O4 Si4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     796.63
_cod_database_code               7042375
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C15(H15), C7(H7), C21(H21), C32(H32), C34(H34), C3AA(H3AA),
 C6AA(H6AA)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C28(H28), C6(H6), C4(H4), C5(H5), C3(H3), C2AA(H2AA), C0AA(H0AA)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C9(H9A,H9B,
 H9C), C22(H22A,H22B,H22C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C20(H20A,H20B,
 H20C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C35(H35A,
 H35B,H35C), C8AA(H8AA,H8AB,H8AC), C7AA(H7AA,H7AB,H7AC), C4AA(H4AA,H4AB,H4AC),
 C5AA(H5AA,H5AB,H5AC)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O4(H4A), O0AA(H0AB)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'