l-Aspartate links for stable sodium metal-organic frameworks.
Siman, Peter; Trickett, Christopher A.; Furukawa, Hiroyasu; Yaghi, Omar M.; Chemical communications (Cambridge, England) 51 (2015) 17463–17466; doi:10.1039/c5cc07578e

data_7118127
_publ_section_title
;
 l-Aspartate links for stable sodium metal-organic frameworks.
;
_journal_issue                   98
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              17463
_journal_page_last               17466
_journal_paper_doi               10.1039/c5cc07578e
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C16.25 H16.11 N2 Na4 O11.86, C0.165 O0.375, 0.37(H2 O), 0.125(O), 0.125(C O)'
_chemical_formula_sum            'C16.54 H16.85 N2 Na4 O12.85'
_chemical_formula_weight         541.29
_chemical_name_common            'MOF-705 after supercritical CO2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-24 deposited with the CCDC.
2015-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.366(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0448(19)
_cell_length_b                   5.2432(5)
_cell_length_c                   16.9833(14)
_cell_measurement_temperature    100(2)
_cell_volume                     2083.1(3)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
Diamond - Crystal and Molecular Structure Visualization
Crystal Impact - Dr. H. Putz & Dr. K. Brandenburg GbR, Kreuzherrenstr. 
102, 53227 Bonn, Germany
http://www.crystalimpact.com/diamond
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.1078
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18857
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        23.300
_diffrn_reflns_theta_max         23.539
_diffrn_reflns_theta_min         2.568
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Bruker,2014/4)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 1129 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         4815
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1092P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1878
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                3270
_reflns_number_total             4815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc07578e2.cif
_cod_data_source_block           MOF-705_sc
_cod_depositor_comments
;

2023-11-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1082.58
_cod_original_formula_moiety
'C32.5 H32.23 N4 Na8 O23.73, C0.33 O0.75, 0.73(H2 O), 0.25(O), 0.25(C O)'
_cod_original_formula_units_Z            2
_cod_original_formula_sum        'C33.08 H33.70 N4 Na8 O25.71'
_cod_database_code               7118127
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.992
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H9A,H9B} of O9, {H17A,H17B} of O17, All C(H,H) groups,
  All C(H,H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  {H25A,H25B} of O25, {H16A,H16B} of O16
2. Uiso/Uaniso restraints and constraints
Uanis(O6B) = Uanis(O6A)
Uanis(C6) = Uanis(C22)
Uanis(C1) = Uanis(C15) = Uanis(C20) = Uanis(C31)
Uanis(C24) = Uanis(C23) = Uanis(C26) = Uanis(C27)
3. Rigid body (RIGU) restrains
 N3, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C5, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O6B)=1-FVAR(1)
 Sof(O6A)=Sof(O25)=Sof(H25A)=Sof(H25B)=Sof(O24)=Sof(H24A)=FVAR(1)
 Fixed Sof: O26(0.75) O27(0.25) C34(0.33333) C33(0.5) H33A(0.5) H33B(0.5)
 H33C(0.5) O28(0.25) C35(0.25)
5.a Free rotating group:
 O25(H25A,H25B)
5.b Rotating group:
 O16(H16A,H16B)
5.c Ternary CH refined with riding coordinates:
 C18(H18), C3(H3A), C13(H13), C29(H29)
5.d Secondary CH2 refined with riding coordinates:
 O9(H9A,H9B), O17(H17A,H17B), C14(H14A,H14B), C19(H19A,H19B), C2(H2A,H2B),
 C30(H30A,H30B)
5.e Me refined with riding coordinates:
 C33(H33A,H33B,H33C)
5.f Aromatic/amide H refined with riding coordinates:
 N3(H3), N1(H1), N2(H2), N4(H4), C11(H11), C27(H27), C23(H23), C10(H10),
 C8(H8), C7(H7), C24(H24), C26(H26)
5.g Tetrahedral OH refined as rotating group:
 O24(H24A)
;
_shelx_res_checksum              15050
_shelx_hkl_checksum              54046