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_7240375
_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         'C48 H58 Cs5.5 Mo10 Na6 O101 P4, H2 O'
_chemical_formula_sum            'C48 H60 Cs5.5 Mo10 Na6 O102 P4'
_chemical_formula_weight         4221.18
_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   mixed
_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
;
2020-02-12 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.491(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0337(7)
_cell_length_b                   16.6107(5)
_cell_length_c                   43.9445(16)
_cell_measurement_reflns_used    9582
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.284
_cell_measurement_theta_min      2.498
_cell_volume                     13867.8(8)
_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      119.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            160607
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.284
_exptl_absorpt_coefficient_mu    2.470
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0849 before and 0.0560 after correction. The Ratio of minimum to maximum transmission is 0.6341. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_description       block
_exptl_crystal_F_000             8050
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.354
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.031(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1626
_refine_ls_number_reflns         24356
_refine_ls_number_restraints     2797
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0563P)^2^+123.3983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                24048
_reflns_number_total             24356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00397b2.cif
_cod_data_source_block           1_a_CCDC1
_cod_original_formula_sum        'C48 H60 Cs5.50 Mo10 Na6 O102 P4'
_cod_database_code               7240375
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.969(12)
 0.031(12)
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 O6 \\sim O7 \\sim O7W \\sim O8 \\sim O8W \\sim O9 \\sim O10 \\sim O10W
\\sim O11 \\sim O11W \\sim O12 \\sim O12W \\sim O13 \\sim O13W \\sim O14 \\sim
O14W \\sim O15 \\sim O9W \\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 O5W \\sim O6W: within 5A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cs5(0.5) Cs6(0.5) Cs7(0.25) Cs8(0.125) Cs9(0.125) Na2(0.5) Na3(0.5)
5.a Riding coordinates:
 C39(H39), C40(H40), C46(H46)
5.b Free rotating group:
 O6W(H6WA,H6WB)
5.c Rotating group:
 O5W(H5WA,H5WB)
5.d Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19),
  C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37),
  C38(H38), C41(H41), C44(H44), C45(H45), C47(H47)
5.e Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C18(H18A,H18B), C28(H28A,H28B), C29(H29A,H29B), C35(H35A,
 H35B), C42(H42A,H42B), C43(H43A,H43B), C48(H48A,H48B)
;
_shelx_res_checksum              20354
_shelx_fab_checksum              65484
_olex2_submission_special_instructions 'No special instructions were received'