Metal‒organic frameworks from novel flexible triptycene- and pentiptycene-based ligands
Crane, Angela K.; Wong, Elaine Y. L.; MacLachlan, Mark J.; CrystEngComm 15 (2013) 9811–; doi:10.1039/c3ce41459k

data_7238861
_publ_section_title
;
 Metal--organic frameworks from novel flexible triptycene- and
 pentiptycene-based ligands
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9811
_journal_paper_doi               10.1039/c3ce41459k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety
'2(C156 H110 N2 O22 Zn4), 12(C3 H7 N O), 5(H2 O)'
_chemical_formula_sum            'C348 H314 N16 O61 Zn8'
_chemical_formula_weight         6219.33
_chemical_name_common            PMOF-1
_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
_audit_creation_date             2013-09-16
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                87.730(5)
_cell_angle_beta                 68.378(5)
_cell_angle_gamma                68.299(5)
_cell_formula_units_Z            1
_cell_length_a                   18.978(5)
_cell_length_b                   23.170(5)
_cell_length_c                   23.477(5)
_cell_measurement_reflns_used    84407
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      24.901
_cell_measurement_theta_min      2.389
_cell_volume                     8861(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1998)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.696
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX DUO'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.696
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            84407
_diffrn_reflns_point_group_measured_fraction_full 0.696
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.267
_diffrn_reflns_theta_min         1.770
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2004
_refine_ls_number_reflns         22294
_refine_ls_number_restraints     441
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0958
_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^)+(0.1464P)^2^+34.9598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2697
_refine_ls_wR_factor_ref         0.2908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14947
_reflns_number_total             22294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce41459k.txt
_cod_data_source_block           mo_mm140_0m
_cod_database_code               7238861
_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
 N2A-C155
 1.5 with sigma of 0.02
3. Restrained planarity
 O21A, C151, N1A, C152, C153
 with sigma of 0.1
 O21B, C251, N1B, C252, C253
 with sigma of 0.1
 O22A, C154, N2A, C155, C156
 with sigma of 0.1
 O22B, C254, N2B, C255, C256
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C156) \\sim Ueq, Uanis(C154) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C155) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C256) \\sim Ueq, Uanis(C255) \\sim Ueq, Uanis(C254) \\sim Ueq, Uanis(N2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C160) \\sim Ueq, Uanis(C163) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O22A) \\sim Ueq, Uanis(O22B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O22A) = Uanis(O22B)
Uanis(N2A) = Uanis(N2B)
Uanis(C154) = Uanis(C254)
Uanis(C155) = Uanis(C255)
Uanis(C156) = Uanis(C256)
Uanis(O21A) = Uanis(O21B)
Uanis(N1A) = Uanis(N1B)
Uanis(C151) = Uanis(C251)
Uanis(C152) = Uanis(C252)
Uanis(C153) = Uanis(C253)
5. Same fragment restrains
{O27, C169, N7, C170, C171}
as
{O21A, C151, N1A, C152, C153}
{O27, C169, N7, C170, C171}
as
{O21B, C251, N1B, C252, C253}
{O27, C169, N7, C170, C171}
as
{O22A, C154, N2A, C155, C156}
{O27, C169, N7, C170, C171}
as
{O22B, C254, N2B, C255, C256}
{O27, C169, N7, C170, C171}
as
{O29, C175, N9, C176, C177}
{O27, C169, N7, C170, C171}
as
{O24, C160, N4, C161, C162}
{O27, C169, N7, C170, C171}
as
{O25, C163, N5, C164, C165}
{O27, C169, N7, C170, C171}
as
{O23, C157, N3, C158, C159}
{O27, C169, N7, C170, C171}
as
{O31, C181, N11, C183, C182}
6. Others
 Sof(O22B)=Sof(C254)=Sof(H254)=Sof(N2B)=Sof(C255)=Sof(H25G)=Sof(H25H)=
 Sof(H25I)=Sof(C256)=Sof(H25J)=Sof(H25K)=Sof(H25L)=1-FVAR(1)
 Sof(O22A)=Sof(C154)=Sof(H154)=Sof(N2A)=Sof(C155)=Sof(H15G)=Sof(H15H)=
 Sof(H15I)=Sof(C156)=Sof(H15J)=Sof(H15K)=Sof(H15L)=FVAR(1)
 Sof(O21B)=Sof(C251)=Sof(H251)=Sof(N1B)=Sof(C252)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=Sof(C253)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(2)
 Sof(O21A)=Sof(C151)=Sof(H151)=Sof(N1A)=Sof(C152)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C153)=Sof(H15D)=Sof(H15E)=Sof(H15F)=FVAR(2)
 Fixed Sof: O34(0.5) O35(0.5) O36(0.5) O37(0.5) O38(0.5)
7.a Ternary CH refined with riding coordinates:
 C55(H55), C56(H56), C71(H71), C72(H72), C5(H5), C6(H6), C21(H21), C22(H22),
 C104(H104), C105(H105), C128(H128), C130(H130)
7.b Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C93(H93A,H93B), C35(H35A,H35B), C43(H43A,H43B), C118(H11A,
 H11B), C143(H14A,H14B)
7.c Me refined with riding coordinates:
 C152(H15A,H15B,H15C), C153(H15D,H15E,H15F), C252(H25A,H25B,H25C), C253(H25D,
 H25E,H25F), C155(H15G,H15H,H15I), C156(H15J,H15K,H15L), C255(H25G,H25H,H25I),
 C256(H25J,H25K,H25L), C170(H17A,H17B,H17C), C171(H17D,H17E,H17F), C176(H17G,
 H17H,H17I), C177(H17J,H17K,H17L), C161(H16A,H16B,H16C), C162(H16D,H16E,H16F),
 C164(H16G,H16H,H16I), C165(H16J,H16K,H16L), C158(H15M,H15N,H15O), C159(H15P,
 H15Q,H15R), C183(H18A,H18B,H18C), C182(H18D,H18E,H18F)
7.d Aromatic/amide H refined with riding coordinates:
 C59(H59), C60(H60), C61(H61), C62(H62), C65(H65), C66(H66), C67(H67),
 C68(H68), C75(H75), C76(H76), C77(H77), C78(H78), C81(H81), C82(H82), C83(H83),
  C84(H84), C87(H87), C88(H88), C90(H90), C91(H91), C95(H95), C96(H96),
 C98(H98), C99(H99), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C18(H18), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32),
  C33(H33), C34(H34), C37(H37), C38(H38), C40(H40), C41(H41), C45(H45),
 C46(H46), C48(H48), C49(H49), C108(H108), C109(H109), C110(H110), C111(H111),
 C114(H114), C115(H115), C116(H116), C117(H117), C120(H120), C121(H121),
 C123(H123), C124(H124), C133(H133), C134(H134), C135(H135), C136(H136),
 C139(H139), C140(H140), C141(H141), C142(H142), C145(H145), C146(H146),
 C148(H148), C149(H149), C151(H151), C251(H251), C154(H154), C254(H254),
 C169(H169), C175(H175), C160(H160), C163(H163), C157(H157), C181(H181)
;
_shelxl_version_number           2013-3