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_7042376
_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_absolute_configuration unk
_chemical_formula_moiety         'C52 H108 Ga4 N4 Si4'
_chemical_formula_sum            'C52 H108 Ga4 N4 Si4'
_chemical_formula_weight         1180.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-14
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6181(6)
_cell_length_b                   18.9494(8)
_cell_length_c                   19.7553(8)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.78
_cell_measurement_theta_min      2.38
_cell_volume                     6221.0(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            153166
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.990
_diffrn_reflns_theta_min         2.325
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0726 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.9173.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.391
_exptl_crystal_size_min          0.307
_refine_diff_density_max         2.251
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
 Flack x determined using 8380 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0059(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         23303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.1560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                20208
_reflns_number_total             23303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00321h1.cif
_cod_data_source_block           ck16_0m
_cod_depositor_comments
'Adding full bibliography for 7042367--7042376.cif.'
_cod_database_code               7042376
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C41)=Sof(H41A)=Sof(H41B)=1-FVAR(1)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N3(H3), N4(H4), N2(H2), N1(H1), C28(H28), C14(H14), C16(H16), C34(H34),
 C22(H22), C19(H19), C25(H25), C31(H31)
3.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C51(H51A,H51B), C4AA(H4AA,H4AB), C39(H39A,H39B), C37(H37A,
 H37B), C45(H45A,H45B), C49(H49A,H49B), C43(H43A,H43B), C41(H41A,H41B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C9(H9), C3(H3A), C11(H11), C6(H6), C8(H8), C5(H5), C12(H12)
3.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C35(H35A,H35B,
 H35C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C29(H29A,H29B,H29C), C13(H13A,
 H13B,H13C), C5AA(H5AA,H5AB,H5AC), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C),
 C40(H40A,H40B,H40C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C), C30(H30A,H30B,
 H30C), C20(H20A,H20B,H20C), C46(H46A,H46B,H46C), C23(H23A,H23B,H23C), C26(H26A,
 H26B,H26C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C38(H38A,H38B,H38C),
 C50(H50A,H50B,H50C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'