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_7118128
_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         'C22 H18 N2 Na4 O12, C0.5 H2.5 O'
_chemical_formula_sum            'C22.5 H20.5 N2 Na4 O13'
_chemical_formula_weight         618.87
_chemical_name_common            'MOF-706 as-synthesized'
_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                 103.886(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0790(15)
_cell_length_b                   5.2419(6)
_cell_length_c                   21.254(3)
_cell_measurement_reflns_used    2395
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.631
_cell_measurement_theta_min      2.218
_cell_volume                     1306.4(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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     0.8856
_diffrn_reflns_av_R_equivalents  0.1134
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7646
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        21.655
_diffrn_reflns_theta_max         21.724
_diffrn_reflns_theta_min         2.164
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1184 before and 0.0852 after correction.
The Ratio of minimum to maximum transmission is 0.8113.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       Needle
_exptl_crystal_F_000             635
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 441 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.8(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         1594
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0721
_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^)+(0.1483P)^2^+0.7645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2093
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                1241
_reflns_number_total             1594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc07578e2.cif
_cod_data_source_block           MOF-706_as
_cod_original_formula_sum        'C22.50 H20.50 N2 Na4 O13'
_cod_database_code               7118128
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.997
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C12-C14A \\sim C14A-C16A \\sim C16A-C12 \\sim C13A-C15 \\sim C15-C17A \\sim
C17A-C13A \\sim C12-C14B
 \\sim C14B-C16B \\sim C16B-C12 \\sim C13B-C15 \\sim C15-C17B \\sim C17B-C13B
 with sigma of 0.02
3. Restrained planarity
 C12, C13A, C14A, C15, C16A, C17A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C1) = Uanis(C4)
Uanis(C5) = Uanis(C18) = Uanis(C15)
Uanis(O8) = Uanis(O9)
Uanis(C13A) = Uanis(C14A) = Uanis(C16A) = Uanis(C17A)
Uanis(C13B) = Uanis(C14B) = Uanis(C16B) = Uanis(C17B)
Uanis(N1) = Uanis(N2)
5. Rigid body (RIGU) restrains
 C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C5, C6, C10, C11, C2, C3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C13A(0.5) H13A(0.5) C14A(0.5) H14A(0.5) C16B(0.5) H16B(0.5)
 C16A(0.5) H16A(0.5) C17B(0.5) H17B(0.5) C17A(0.5) H17A(0.5) C13B(0.5)
 H13B(0.5) C14B(0.5) H14B(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
7.a Ternary CH refined with riding coordinates:
 C3(H3), C19(H19)
7.b Secondary CH2 refined with riding coordinates:
 O12(H12A,H12B), C21(H21A,H21B), C2(H2A,H2B)
7.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C7(H7), C10(H10), C8(H8), C11(H11), C13A(H13A), C14A(H14A),
 C16B(H16B), C16A(H16A), C17B(H17B), C17A(H17A), C13B(H13B), C14B(H14B)
7.d Tetrahedral OH refined with riding coordinates:
 O13(H13)
7.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              68788
_shelx_hkl_checksum              78882