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_7240377
_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 H112 Mo20 Na23 O209.5 P8, H2 O'
_chemical_formula_sum            'C96 H114 Mo20 Na23 O210.5 P8'
_chemical_formula_weight         7331.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-12
_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                 92.424(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   44.727(3)
_cell_length_b                   17.6015(10)
_cell_length_c                   32.7474(18)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.57
_cell_volume                     25758(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      119.95
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            423375
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.867
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.4539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1061 before and 0.0757 after correction. The Ratio of minimum to maximum transmission is 0.8058. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_description       block
_exptl_crystal_F_000             14348
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.273
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3236
_refine_ls_number_reflns         45126
_refine_ls_number_restraints     16927
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+419.5275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1412
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                44587
_reflns_number_total             45126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00397b2.cif
_cod_data_source_block           1_a_CCDC2
_cod_original_formula_sum        'C96 H114 Mo20 Na23 O210.50 P8'
_cod_database_code               7240377
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.762
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(3)
 0.06(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,H) groups
3. Uiso/Uaniso restraints and constraints
O1 \\sim O1W \\sim O2 \\sim O2W \\sim O3 \\sim O3W \\sim O4 \\sim O4W \\sim O5
\\sim O5W \\sim O6 \\sim O6W \\sim O7 \\sim O7W \\sim O8 \\sim O8W \\sim O9
\\sim O9W \\sim O10 \\sim O10W \\sim O11 \\sim O11W \\sim O12 \\sim O12W \\sim
O13 \\sim O13W \\sim O14 \\sim O14W \\sim O15 \\sim O15W \\sim O16 \\sim O16W
\\sim O17 \\sim O17W \\sim O18 \\sim O18W \\sim O19 \\sim O19W \\sim O20 \\sim
O20W \\sim O21 \\sim O21W \\sim O22 \\sim O22W \\sim O23 \\sim O23W \\sim O24
\\sim O24W \\sim O25 \\sim O25W \\sim O26 \\sim O26W \\sim O27 \\sim O27W \\sim
O28 \\sim O28W \\sim O29 \\sim O29W \\sim O30 \\sim O30W \\sim O31 \\sim O31W
\\sim O32 \\sim O32W \\sim O33 \\sim O33W \\sim O34 \\sim O34W \\sim O35 \\sim
O35W \\sim O36 \\sim O36W \\sim O37 \\sim O38 \\sim O40W \\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 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 O37W \\sim O38W \\sim
O39W \\sim O135 \\sim P1 \\sim P2 \\sim P3 \\sim P4 \\sim P5 \\sim P6 \\sim P7
\\sim P8: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02
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 C18 \\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: within
5A with sigma of 0.01 and sigma for terminal atoms of 0.02
Na1 \\sim Na2 \\sim Na3 \\sim Na4 \\sim Na5 \\sim Na6 \\sim Na7 \\sim Na8 \\sim
Na9 \\sim Na10 \\sim Na11 \\sim Na12 \\sim Na13 \\sim Na14 \\sim Na15 \\sim
Na16 \\sim Na17 \\sim Na18 \\sim Na19 \\sim Na20 \\sim Na21 \\sim Na22 \\sim
Na23: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02
O170 \\sim C95 \\sim C94 \\sim O134 \\sim C45 \\sim C46 \\sim C39 \\sim C86
\\sim O133 \\sim C40 \\sim O167 \\sim C87 \\sim C44 \\sim C41 \\sim C43 \\sim
C42 \\sim O164 \\sim O161 \\sim O160 \\sim C80 \\sim C81 \\sim O162 \\sim C84
\\sim C85 \\sim O163 \\sim C83 \\sim C82 \\sim O159 \\sim O158 \\sim C93 \\sim
O157 \\sim O156 \\sim C89 \\sim C88 \\sim C91 \\sim O171 \\sim C90 \\sim C78
\\sim O153 \\sim O155 \\sim C76 \\sim O154 \\sim C77 \\sim C75 \\sim C79 \\sim
O150 \\sim C73 \\sim C74 \\sim O151 \\sim O149 \\sim O147 \\sim O148 \\sim C67
\\sim O146 \\sim C65 \\sim C33 \\sim C32 \\sim C68 \\sim O145 \\sim O144 \\sim
O140 \\sim O135 \\sim C69 \\sim C35 \\sim O143 \\sim C64 \\sim C34 \\sim C38
\\sim O141 \\sim C36 \\sim O139 \\sim C37 \\sim O136 \\sim C71 \\sim C72 \\sim
C70 \\sim C92 \\sim O138 \\sim O137 \\sim O132 \\sim O131 \\sim O130 \\sim O165
\\sim O142 \\sim O152: within 5A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O119 \\sim O118 \\sim C22 \\sim C53 \\sim C19 \\sim O120 \\sim C20 \\sim O117
\\sim C21 \\sim O115 \\sim C23 \\sim C24 \\sim O112 \\sim C25 \\sim C26 \\sim
C27 \\sim O114 \\sim O110 \\sim C28 \\sim C30 \\sim C31 \\sim O107 \\sim C29
\\sim O109 \\sim O106 \\sim C15 \\sim C50 \\sim O108 \\sim O105 \\sim C49 \\sim
O101 \\sim C48 \\sim C18 \\sim C17 \\sim O102 \\sim O104 \\sim C47 \\sim O103
\\sim O100 \\sim C59 \\sim C57 \\sim C58 \\sim O172 \\sim C60 \\sim O169 \\sim
C61 \\sim C14 \\sim O99 \\sim O168 \\sim O98 \\sim C13 \\sim C63 \\sim O96
\\sim O95 \\sim C62 \\sim C11 \\sim C12 \\sim O94 \\sim O93 \\sim C10 \\sim O97
\\sim C3 \\sim C4 \\sim O126 \\sim C9 \\sim C2 \\sim O128 \\sim C1 \\sim C5
\\sim O127 \\sim O129 \\sim O123 \\sim C6 \\sim C7 \\sim O124 \\sim C55 \\sim
O121 \\sim C54 \\sim O122 \\sim C56 \\sim C8 \\sim O125 \\sim C52 \\sim O116
\\sim C51 \\sim O111 \\sim C16: within 5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Na22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O25W(0.5) O38W(0.5) O39W(0.5)
5.a Free rotating group:
 O37W(H37A,H37B)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10),
 C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
  C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43),
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C53(H53), C55(H55),
  C56(H56), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63),
 C64(H64), C65(H65), C66(H66), C67(H67), C70(H70), C71(H71), C73(H73), C74(H74),
  C75(H75), C76(H76), C77(H77), C78(H78), C80(H80), C81(H81), C82(H82),
 C83(H83), C84(H84), C86(H86), C87(H87), C88(H88), C90(H90), C91(H91), C92(H92),
  C93(H93), C94(H94), C96(H96)
5.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C31(H31A,H31B), C42(H42A,H42B), C49(H49A,H49B),
 C51(H51A,H51B), C52(H52A,H52B), C54(H54A,H54B), C58(H58A,H58B), C68(H68A,H68B),
  C69(H69A,H69B), C72(H72A,H72B), C79(H79A,H79B), C85(H85A,H85B), C89(H89A,
 H89B), C95(H95A,H95B)
;
_shelx_res_checksum              23776
_shelx_fab_checksum              64511
_olex2_submission_special_instructions 'No special instructions were received'