Intrinsically porous molecular building blocks for metal organic frameworks tailored by the bridging effect of counter cations
Yang, Peng; Alshankiti, Buthainah; Khashab, Niveen M.; CrystEngComm  (2020) –; doi:10.1039/D0CE00397B

data_7240378
_publ_section_title
;
 Intrinsically porous molecular building blocks for metal organic
 frameworks tailored by the bridging effect of counter cations
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00397B
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C96 H110 K20 Mo20 Na1.5 O193 P8'
_chemical_formula_sum            'C96 H110 K20 Mo20 Na1.5 O193 P8'
_chemical_formula_weight         7334.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-12 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.956(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.048(2)
_cell_length_b                   16.1202(9)
_cell_length_c                   47.517(3)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.50
_cell_volume                     25609(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0357
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            396465
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.876
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.4977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1204 before and 0.0536 after correction. The Ratio of minimum to maximum transmission is 0.8835. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       block
_exptl_crystal_F_000             14346
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.244
_refine_diff_density_min         -2.062
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3091
_refine_ls_number_reflns         45079
_refine_ls_number_restraints     14615
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+529.6580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                44527
_reflns_number_total             45079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00397b2.cif
_cod_data_source_block           1_a_CCDC4
_cod_original_formula_sum        'C96 H110 K20 Mo20 Na1.50 O193 P8'
_cod_database_code               7240378
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.707
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93(3)
 0.07(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C94-H75
 1.5 with sigma of 0.02
 C75-C94
 0.01 with sigma of 1.6
 C76-C73
 1.52 with sigma of 0.02
 C73-C74
 1.52 with sigma of 0.02
 C94-C75
 1.52 with sigma of 0.02
 O66-C75
 1.44 with sigma of 0.02
 C96-O66
 1.44 with sigma of 0.02
 C94-O67
 1.44 with sigma of 0.02
 C74-C96
 1.45 with sigma of 0.02
 C75-C76
 1.46 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26
\\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34
\\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42
\\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50
\\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58
\\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66
\\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74
\\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82
\\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90
\\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C18: within
5A with sigma of 0.01 and sigma for terminal atoms of 0.02
K1 \\sim K2 \\sim K3 \\sim K4 \\sim K5 \\sim K6 \\sim K7 \\sim K8 \\sim K9
\\sim K10 \\sim K11 \\sim K12 \\sim K13 \\sim K14 \\sim K15 \\sim K16 \\sim K17
\\sim K18 \\sim K19A \\sim K20 \\sim K21 \\sim K19B: within 5A with sigma of
0.01 and sigma for terminal atoms of 0.02
Na1 \\sim Na2: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O16 \\sim O17 \\sim O18
\\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim O26
\\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim O34
\\sim O35 \\sim O36 \\sim O37 \\sim O38 \\sim O39 \\sim O40 \\sim O41 \\sim O42
\\sim O43 \\sim O44 \\sim O45 \\sim O46 \\sim O47 \\sim O48 \\sim O49 \\sim O50
\\sim O51 \\sim O52 \\sim O53 \\sim O54 \\sim O55 \\sim O56 \\sim O57 \\sim O58
\\sim O59 \\sim O60 \\sim O61 \\sim O62 \\sim O63 \\sim O64 \\sim O65 \\sim O66
\\sim O67 \\sim O68 \\sim O69 \\sim O70 \\sim O71 \\sim O72 \\sim O73 \\sim O74
\\sim O75 \\sim O76 \\sim O77 \\sim O78 \\sim O79 \\sim O80 \\sim O81 \\sim O82
\\sim O83 \\sim O84 \\sim O85 \\sim O86 \\sim O87 \\sim O88 \\sim O89 \\sim O90
\\sim O91 \\sim O92 \\sim O93 \\sim O94 \\sim O95 \\sim O96 \\sim O97 \\sim O98
\\sim O99 \\sim O100 \\sim O101 \\sim O102 \\sim O103 \\sim O104 \\sim O105
\\sim O106 \\sim O107 \\sim O108 \\sim O109 \\sim O110 \\sim O111 \\sim O112
\\sim O113 \\sim O114 \\sim O115 \\sim O116 \\sim O117 \\sim O118 \\sim O119
\\sim O120 \\sim O121 \\sim O122 \\sim O123 \\sim O124 \\sim O125 \\sim O126
\\sim O127 \\sim O128 \\sim O129 \\sim O130 \\sim O131 \\sim O132 \\sim O133
\\sim O134 \\sim O135 \\sim O136 \\sim O137 \\sim O138 \\sim O139 \\sim O140
\\sim O141 \\sim O142 \\sim O143 \\sim O144 \\sim O145 \\sim O146 \\sim O147
\\sim O148 \\sim O149 \\sim O150 \\sim O151 \\sim O152 \\sim O153 \\sim O154
\\sim O155 \\sim O156 \\sim O157 \\sim O158 \\sim O159 \\sim O160 \\sim O161
\\sim O162 \\sim O163 \\sim O164 \\sim O165 \\sim O166 \\sim O167 \\sim O168
\\sim O169 \\sim O170 \\sim O171 \\sim O172 \\sim O173 \\sim O174 \\sim O19W
\\sim O1W \\sim O2W \\sim O3W \\sim O4W \\sim O5W \\sim O6W \\sim O7W \\sim O8W
\\sim O9W \\sim O10W \\sim O11W \\sim O12W \\sim O13W \\sim O16W \\sim O17W
\\sim O18W \\sim O20W \\sim O15W \\sim O14W \\sim O21W \\sim O15: within 5A
with sigma of 0.01 and sigma for terminal atoms of 0.01
O63 \\sim C73 \\sim C74 \\sim O64 \\sim C96 \\sim O66 \\sim C75 \\sim C94 \\sim
O67 \\sim C76 \\sim O68 \\sim C78 \\sim C82 \\sim O71 \\sim O72 \\sim C81 \\sim
C80 \\sim O69 \\sim C79 \\sim O73 \\sim C83 \\sim O70 \\sim C89 \\sim O74 \\sim
O75 \\sim C90 \\sim C91 \\sim O76 \\sim C93 \\sim C92 \\sim C95 \\sim O77 \\sim
O82 \\sim C84 \\sim O81 \\sim C87 \\sim C88 \\sim O80 \\sim O65 \\sim C77 \\sim
C86 \\sim C85 \\sim O79 \\sim O78: within 5A with sigma of 0.01 and sigma for
terminal atoms of 0.01
C17 \\sim O16 \\sim C16 \\sim C21 \\sim O12 \\sim O14 \\sim C15 \\sim C13 \\sim
C14 \\sim O18 \\sim O21 \\sim O11 \\sim C6 \\sim O20 \\sim C7 \\sim C24 \\sim
C22 \\sim O17 \\sim O19 \\sim O7 \\sim C4 \\sim C5 \\sim C10 \\sim C3 \\sim O9
\\sim C2 \\sim C1 \\sim O10 \\sim O3 \\sim O8 \\sim C9 \\sim C8 \\sim O2 \\sim
C12 \\sim O1 \\sim O5 \\sim O4 \\sim C11 \\sim C23 \\sim O6 \\sim C19 \\sim C20
\\sim O13 \\sim C18 \\sim O15: within 5A with sigma of 0.01 and sigma for
terminal atoms of 0.01
O62 \\sim C72 \\sim C58 \\sim O52 \\sim C60 \\sim C69 \\sim O51 \\sim C57 \\sim
C56 \\sim O50 \\sim C55 \\sim O49 \\sim O48 \\sim O47 \\sim C49 \\sim C53 \\sim
C52 \\sim C54 \\sim O43 \\sim O44 \\sim O45 \\sim C51 \\sim C66 \\sim C50 \\sim
C71 \\sim O61 \\sim O46 \\sim O53 \\sim C59 \\sim C70 \\sim C63 \\sim C62 \\sim
O55 \\sim O54 \\sim C61 \\sim O57 \\sim C64 \\sim C67 \\sim O60 \\sim O58 \\sim
C65 \\sim C68 \\sim O59: within 5A with sigma of 0.01 and sigma for terminal
atoms of 0.01
O33 \\sim C44 \\sim O31 \\sim C41 \\sim C39 \\sim O27 \\sim C40 \\sim O32 \\sim
O34 \\sim C42 \\sim C43 \\sim O38 \\sim C37 \\sim C35 \\sim C47 \\sim O39 \\sim
O42 \\sim O35 \\sim C36 \\sim O37 \\sim O36 \\sim C38 \\sim C34 \\sim C48 \\sim
O40 \\sim O25 \\sim C26 \\sim C25 \\sim O26 \\sim C27 \\sim O22 \\sim O23 \\sim
O24 \\sim C29 \\sim C28 \\sim C45 \\sim O41 \\sim C31 \\sim C30 \\sim O30 \\sim
C46 \\sim C33 \\sim O28 \\sim C32 \\sim O29: within 5A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(K19A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: O11(0.5) O21(0.5) O39(0.5) O42(0.5) K19A(0.5) K20(0.5) K21(0.5)
 Na2(0.5) K19B(0.5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
  C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
 C46(H46), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56),
  C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63),
 C64(H64), C65(H65), C66(H66), C67(H67), C69(H69), C71(H71), C73(H73), C74(H74),
  C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81),
 C82(H82), C84(H84), C85(H85), C86(H86), C87(H87), C89(H89), C90(H90), C91(H91),
  C92(H92), C93(H93), C96(H96)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C23(H23A,H23B), C44(H44A,H44B), C45(H45A,H45B), C48(H48A,
 H48B), C54(H54A,H54B), C68(H68A,H68B), C70(H70A,H70B), C72(H72A,H72B),
 C83(H83A,H83B), C88(H88A,H88B), C94(H94A,H94B), C95(H95A,H95B), C18(H18A,H18B)
6.c Idealised tetrahedral OH refined as rotating group:
 O67(H67A), O15(H15A)
;
_shelx_res_checksum              48960
_shelx_fab_checksum              79896
_olex2_submission_special_instructions 'No special instructions were received'