Clathrate directed assembly of tetrapyridyl-tetraphenylethylene metal‒organic frameworks
Jackson, Sam L.; Rananaware, Anushri; Rix, Colin; Bhosale, Sheshanath V.; Latham, Kay; RSC Advances 5 (2015) 84134–; doi:10.1039/C5RA18499A

data_7235994
_publ_section_title
;
 Clathrate directed assembly of tetrapyridyl-tetraphenylethylene
 metal--organic frameworks
;
_journal_issue                   102
_journal_name_full               'RSC Advances'
_journal_page_first              84134
_journal_paper_doi               10.1039/C5RA18499A
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C46 H32 Cl2 Cu N4, 4(C2 Cl4)'
_chemical_formula_sum            'C54 H32 Cl18 Cu N4'
_chemical_formula_weight         1438.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-A 2ab 2b'
_space_group_name_H-M_alt        'A c a a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-13 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.675(3)
_cell_length_b                   29.299(4)
_cell_length_c                   34.539(4)
_cell_measurement_temperature    200(2)
_cell_volume                     23958(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'APEX II CCD detector'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1778
_diffrn_reflns_av_unetI/netI     0.0996
_diffrn_reflns_Laue_measured_fraction_full 0.872
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            91110
_diffrn_reflns_point_group_measured_fraction_full 0.872
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         24.761
_diffrn_reflns_theta_min         1.253
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.209
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plates
_exptl_crystal_F_000             11504.0
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method layering
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         10274
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.2173
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1384P)^2^+90.3100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2286
_refine_ls_wR_factor_ref         0.3088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3868
_reflns_number_total             9755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra18499a2.cif
_cod_data_source_block           CuCl2tppe4TCE
_cod_original_sg_symbol_Hall     '-A 2ac 2c'
_cod_original_sg_symbol_H-M      'A c a a'
_cod_database_code               7235994
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C50-C49 \\sim C48-C47 \\sim C52-C51 \\sim C54-C53
 with sigma of 0.02
3. Rigid bond restraints
 C47, C48, C50, C49, C52, C51, C54, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C49 \\sim C50 \\sim C48 \\sim C47 \\sim C51 \\sim C52 \\sim C53 \\sim C54:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
N3 \\sim N4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C24 \\sim C44: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C45 \\sim C28: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C27(H27), C28(H28), C30(H30), C31(H31), C33(H33), C34(H34),
 C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              25351
_olex2_submission_special_instructions 'No special instructions were received'