Framework complexes of group 2 metals organized by homochiral rods and π···π stacking forces: a breathing supramolecular MOF.
Reger, Daniel L.; Leitner, Andrew; Pellechia, Perry J.; Smith, Mark D.; Inorganic chemistry 53 (2014) 9932–9945; doi:10.1021/ic501581c

data_4340950
_publ_section_title
;
 Framework complexes of group 2 metals organized by homochiral rods and
 \p&#x00B7;&#x00B7;&#x00B7;\p stacking forces: a breathing supramolecular
 MOF.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9932
_journal_page_last               9945
_journal_paper_doi               10.1021/ic501581c
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H20 N2 O9 Sr, 3.33(H2 O)'
_chemical_formula_sum            'C30 H28.66 N2 O12.33 Sr'
_chemical_formula_weight         702.09
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.9232(12)
_cell_length_b                   19.9232(12)
_cell_length_c                   14.9716(18)
_cell_measurement_reflns_used    8334
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.040
_cell_measurement_theta_min      2.286
_cell_volume                     5942.7(9)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.631 (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            87185
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.421
_diffrn_reflns_theta_min         1.445
_diffrn_source                   'Sealed tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2874
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 2157 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.021(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0760P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5395
_reflns_number_total             6103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501581c_si_002.cif
_cod_data_source_block           3rehydrated
_cod_depositor_comments
'Adding full bibliography for 4340945--4340952.cif.'
_cod_original_cell_volume        5942.7(10)
_cod_database_code               4340950
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{O7A, O7B}
{O8A, O8B}
3. Uiso/Uaniso restraints and constraints
Uanis(O7A) = Uanis(O7B)
Uanis(O8A) = Uanis(O8B)
Uiso(C28A) = Uiso(C28B)
Uiso(C30A) = Uiso(C30B)
Uiso(O4S) = Uiso(O5S) = Uiso(O1S) = Uiso(O2S) = Uiso(O3S) = Uiso(O6S) =
Uiso(O7S)
Uiso(C29A) = Uiso(C29B)
Uiso(N2A) = Uiso(N2B)
Uiso(C17A) = Uiso(C17B)
4. Same fragment restrains
{O1, O2, O3, O4, N1, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13,
C14, C15}
as
{O5A, O6A, O7A, O8A, N2A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A,
C25A, C26A, C27A, C28A, C29A, C30A}
{O1, O2, O3, O4, N1, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13,
C14, C15}
as
{O5B, O6B, O7B, O8B, N2B, C16B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C24B,
C25B, C26B, C27B, C28B, C29B, C30B}
5. Others
 Sof(O5B)=Sof(O6B)=Sof(O7B)=Sof(O8B)=Sof(N2B)=Sof(C16B)=Sof(C17B)=Sof(C18B)=
 Sof(C19B)=Sof(C20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=
 Sof(H23B)=Sof(C24B)=Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=
 Sof(H27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C30B)=Sof(O3S)=1-FVAR(1)
 Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(N2A)=Sof(C16A)=Sof(C17A)=Sof(C18A)=
 Sof(C19A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=
 Sof(H23A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30A)=Sof(O1S)=FVAR(1)
 Fixed Uiso: O1S(0.05) O2S(0.05) O3S(0.05) O4S(0.05) O5S(0.05) O6S(0.05)
 O7S(0.05) O8S(0.05) O9S(0.05)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C28A(H28A), C28B(H28B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C21A(H21A), C22A(H22A),
 C23A(H23A), C25A(H25A), C26A(H26A), C27A(H27A), C21B(H21B), C22B(H22B),
 C23B(H23B), C25B(H25B), C26B(H26B), C27B(H27B)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F)
;