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_7240374
_publ_section_title
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 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         'C72 H72 Cs4.5 Mo10 Na2.5 O110.5 P4'
_chemical_formula_sum            'C72 H72 Cs4.5 Mo10 Na2.5 O110.5 P4'
_chemical_formula_weight         4444.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-11 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4079(8)
_cell_length_b                   22.3318(10)
_cell_length_c                   43.2705(19)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.276
_cell_measurement_theta_min      2.256
_cell_volume                     15855.1(13)
_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      120.01
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            400360
_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         2.206
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.938
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.3907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1273 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.6936. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_description       block
_exptl_crystal_F_000             8572
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.524
_refine_diff_density_min         -1.636
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.053(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1919
_refine_ls_number_reflns         27824
_refine_ls_number_restraints     5397
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+96.3455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                27525
_reflns_number_total             27824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00397b2.cif
_cod_data_source_block           1_a
_cod_original_formula_sum        'C72 H72 Cs4.50 Mo10 Na2.50 O110.50 P4'
_cod_database_code               7240374
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.675
_shelx_estimated_absorpt_t_min   0.664
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.947(18)
 0.053(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C12-C13
 1.52 with sigma of 0.02
 C9-C8
 1.52 with sigma of 0.02
 C8-O14
 1.35 with sigma of 0.02
 O111-C72
 1.35 with sigma of 0.02
 O112-C72
 1.35 with sigma of 0.02
 C29-C28
 1.53 with sigma of 0.02
 C29-O44
 1.35 with sigma of 0.02
 C38-O60
 1.35 with sigma of 0.02
 C38-C39
 1.56 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
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 O15 \\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 O5W \\sim O3W \\sim O2W \\sim O1W \\sim O106 \\sim O107 \\sim
O108 \\sim O109 \\sim O110 \\sim O111 \\sim O112 \\sim O4W: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.01
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: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C1 \\sim O2 \\sim C4 \\sim C3 \\sim C2 \\sim O4 \\sim O110 \\sim O5 \\sim C7
\\sim O8 \\sim C6 \\sim C5 \\sim O12 \\sim O10 \\sim C10 \\sim C9 \\sim C8
\\sim O14 \\sim O106 \\sim O15 \\sim C13 \\sim O22 \\sim C12 \\sim C11 \\sim
O20 \\sim O18 \\sim C15 \\sim C14 \\sim C16 \\sim C17 \\sim O30 \\sim C18 \\sim
O28 \\sim C19 \\sim O32 \\sim O25 \\sim C22 \\sim C23 \\sim O40 \\sim O38 \\sim
C24 \\sim C25 \\sim O35 \\sim C21 \\sim C20 \\sim O34: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.01
O58 \\sim C36 \\sim C37 \\sim O105 \\sim O52 \\sim C33 \\sim C32 \\sim O50
\\sim C34 \\sim C35 \\sim O55 \\sim C30 \\sim C31 \\sim O48 \\sim O46 \\sim C27
\\sim C26 \\sim O42 \\sim C28 \\sim C29 \\sim O44: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.01
O94 \\sim O95 \\sim C66 \\sim C65 \\sim O93 \\sim C64 \\sim C63 \\sim C62 \\sim
O92 \\sim O96 \\sim C67 \\sim O97 \\sim C69 \\sim C70 \\sim O99 \\sim O100
\\sim C71 \\sim O98 \\sim C68 \\sim C72 \\sim O112 \\sim O111: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.01
O101 \\sim C61 \\sim C60 \\sim O91 \\sim O88 \\sim C57 \\sim C58 \\sim O89
\\sim O90 \\sim C59 \\sim C56 \\sim O87 \\sim O108 \\sim C55 \\sim O85 \\sim
C54 \\sim O80 \\sim C51 \\sim C50 \\sim C49 \\sim O78 \\sim O109 \\sim O82
\\sim O84 \\sim C53 \\sim C52 \\sim O75 \\sim C48 \\sim O70 \\sim C45 \\sim C43
\\sim C44 \\sim O107 \\sim C46 \\sim O72 \\sim C47 \\sim O65 \\sim C42 \\sim
O64 \\sim O74 \\sim O62 \\sim C41 \\sim C40 \\sim C39 \\sim O60 \\sim C38:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cs7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: Cs4(0.5) Cs5(0.5) O4(0.5) O14(0.5) O68(0.5) O78(0.5) O87(0.5)
 Cs6(0.25) Cs7(0.25) Na3(0.5) O1W(0.5) O106(0.5) O107(0.5) O108(0.5) O109(0.5)
 O110(0.5) O111(0.5) O112(0.5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21),
  C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39),
  C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65),
 C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C20(H20A,H20B), C29(H29A,H29B), C35(H35A,H35B), C38(H38A,
 H38B), C62(H62A,H62B)
;
_shelx_res_checksum              97204
_shelx_fab_checksum              33404
_olex2_submission_special_instructions 'No special instructions were received'