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_7235996
_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
'C12 H8 Cl2 Mn N4, 2(C3), 11(C0.50 H0.50), 2(C2), 2(C0.50 H0.50)'
_chemical_formula_sum            'C62.54 H63.32 Cl2 Mn N4'
_chemical_formula_weight         996.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.061(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5708(13)
_cell_length_b                   12.2088(12)
_cell_length_c                   17.3624(17)
_cell_measurement_temperature    200(2)
_cell_volume                     3088.6(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(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29104
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         1.668
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       plates
_exptl_crystal_F_000             1051.1
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8892
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0522
_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^)+(0.1162P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5156
_reflns_number_total             9013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra18499a2.cif
_cod_data_source_block           Mn_tppe_DMB
_cod_database_code               7235996
_shelxl_version_number           2013-4
_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
2. Shared sites
{C17, C17A}
{C20, C20A}
{C6, C6A}
{C9, C9A}
3. Restrained distances
 Mn1-N2 \\sim Mn1-N2A
 with sigma of 0.001
 C3-C6 \\sim C3A-C6A \\sim C14-C17 \\sim C14A-C17A
 with sigma of 0.001
 Mn1-N1 \\sim Mn1-N1A
 with sigma of 0.001
 C3A-C2A \\sim C4-C3
 with sigma of 0.02
 C9A-C10A \\sim C9-C10
 with sigma of 0.02
 C6-C11 \\sim C6A-C11A
 with sigma of 0.02
 C21-C20 \\sim C21A-C20A
 with sigma of 0.02
 C20A-C19A \\sim C20-C19
 with sigma of 0.02
 C1F-C1K \\sim C1L-C1G \\sim C1I-C1J \\sim C1M-C1H
 with sigma of 0.02
4. Restrained planarity
 N1A, C1A, C2A, C3A, C4A, C5A
 with sigma of 0.001
 C10A, C9A, C8A, C7A, C11A, C6A
 with sigma of 0.1
 C18A, C22A, C21A, C19A, C20A, C17A
 with sigma of 0.1
 N2A, C12A, C13A, C14A, C15A, C16A
 with sigma of 0.001
 C1H, C1D, C1B, C1J, C1I, C1M
 with sigma of 0.1
 C1G, C1C, C1E, C1K, C1F, C1L
 with sigma of 0.1
5. Rigid bond restraints
 N1A, C1A, C2A, C3A, C4A, C5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8A, C9A, C10A, C11A, C6A, C7A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18A, C22A, C21A, C19A, C20A, C17A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
N1A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C8A \\sim C9A \\sim C10A \\sim C11A \\sim C6A \\sim C7A: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C18A \\sim C22A \\sim C21A \\sim C19A \\sim C20A \\sim C17A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C19 \\sim C18 \\sim C18A \\sim C19A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
C16A \\sim C15A \\sim C14A \\sim C13A \\sim C12A \\sim N2: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C16A \\sim C15A \\sim C14A \\sim C13A \\sim C12A \\sim N2A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C1M \\sim C1B \\sim C1D \\sim C1I \\sim C1J \\sim C1H: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C1K \\sim C1E \\sim C1F \\sim C1L \\sim C1C \\sim C1G: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C9) = Uanis(C9A)
Uanis(C6) = Uanis(C6A)
Uanis(C17) = Uanis(C17A)
Uanis(C20) = Uanis(C20A)
Uanis(N2) = Uanis(N2A)
Uanis(C14) = Uanis(C14A)
Uanis(C3) = Uanis(C3A)
Uanis(N1) = Uanis(N1A)
7. Others
 Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C9A)=Sof(N2A)=Sof(C14A)=Sof(C17A)=Sof(C20A)=1-
 FVAR(1)
 Sof(N1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5)=Sof(C6)=Sof(C9)=Sof(N2)=Sof(C14)=Sof(C17)=Sof(C20)=FVAR(1)
 Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(H1FC)=FVAR(2)
 Sof(C1G)=Sof(H1GA)=Sof(H1GB)=Sof(H1GC)=FVAR(3)
 Sof(C1K)=Sof(H1KA)=Sof(H1KB)=Sof(H1KC)=FVAR(4)
 Sof(C1I)=Sof(H1IA)=Sof(H1IB)=Sof(H1IC)=FVAR(5)
 Sof(C1J)=Sof(H1JA)=Sof(H1JB)=Sof(H1JC)=FVAR(6)
 Sof(C1M)=Sof(H1MA)=Sof(H1MB)=Sof(H1MC)=FVAR(7)
 Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)=FVAR(8)
 Sof(C1L)=Sof(H1LA)=Sof(H1LB)=Sof(H1LC)=FVAR(9)
 Fixed Sof: C7(0.75) H7(0.75) C8(0.75) H8(0.75) C10(0.75) H10(0.75) C11(0.75)
 H11(0.75) C7A(0.25) H7A(0.25) C8A(0.25) H8A(0.25) C10A(0.25) H10A(0.25)
 C11A(0.25) H11A(0.25) C12(0.75) H12(0.75) C13(0.75) H13(0.75) C15(0.75)
 H15(0.75) C16(0.75) H16(0.75) C12A(0.25) H12A(0.25) C13A(0.25) H13A(0.25)
 C15A(0.25) H15A(0.25) C16A(0.25) H16A(0.25) C18(0.75) H18(0.75) C19(0.75)
 H19(0.75) C21(0.75) H21(0.75) C22(0.75) H22(0.75) C18A(0.25) H18A(0.25)
 C19A(0.25) H19A(0.25) C21A(0.25) H21A(0.25) C22A(0.25) H22A(0.25)
8.a Me refined with riding coordinates:
 C1J(H1JA,H1JB,H1JC), C1L(H1LA,H1LB,H1LC)
8.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C1A(H1A), C2A(H2A), C4A(H4A), C5A(H5A),
 C7(H7), C8(H8), C10(H10), C11(H11), C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A),
  C12(H12), C13(H13), C15(H15), C16(H16), C12A(H12A), C13A(H13A), C15A(H15A),
 C16A(H16A), C18(H18), C19(H19), C21(H21), C22(H22), C18A(H18A), C19A(H19A),
 C21A(H21A), C22A(H22A)
8.c Idealised Me refined as rotating group:
 C1G(H1GA,H1GB,H1GC), C1I(H1IA,H1IB,H1IC), C1M(H1MA,H1MB,H1MC), C1H(H1HA,H1HB,
 H1HC), C1F(H1FA,H1FB,H1FC), C1K(H1KA,H1KB,H1KC)
;
_shelx_res_checksum              47055
_olex2_submission_special_instructions 'No special instructions were received'