Single-Crystal-to-Single-Crystal Postsynthetic Modification of a Metal-Organic Framework via Ozonolysis.
Albalad, Jorge; Xu, Heng; Gándara, Felipe; Haouas, Mohamed; Martineau-Corcos, Charlotte; Mas-Ballesté, Rubén; Barnett, Sarah A.; Juanhuix, Judith; Imaz, Inhar; Maspoch, Daniel; Journal of the American Chemical Society 140 (2018) 2028–2031; doi:10.1021/jacs.7b12913

data_4131910
_publ_section_title
;
 Single-Crystal-to-Single-Crystal Postsynthetic Modification of a
 Metal-Organic Framework via Ozonolysis.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2028
_journal_page_last               2031
_journal_paper_doi               10.1021/jacs.7b12913
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.5(C88 H9.2 O73.6 Zr12), 2.57(O3)'
_chemical_formula_sum            'C44 H4.6 O44.5 Zr6'
_chemical_formula_weight         1792.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 135.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.747(4)
_cell_length_b                   20.747(4)
_cell_length_c                   14.670(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4465(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_wavelength     0.6199
_diffrn_reflns_av_R_equivalents  0.1047
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68694
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        21.835
_diffrn_reflns_theta_max         36.109
_diffrn_reflns_theta_min         1.483
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.010
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             1729
_refine_diff_density_max         3.193
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details
;
 Flack x determined using 7775 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.461(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         27598
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0820P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.782
_reflns_number_gt                21341
_reflns_number_total             27598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12913_si_004.cif
_cod_data_source_block           c2m
_cod_original_cell_volume        4465(2)
_cod_original_formula_sum        'C44 H4.60 O44.50 Zr6'
_cod_database_code               4131910
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Restrained distances
 C10-C3
 1.7 with sigma of 0.02
 C1-C15
 1.7 with sigma of 0.02
 C12-C9
 1.7 with sigma of 0.02
 C4AA-C14
 1.7 with sigma of 0.02
 C0AA-C1B
 1.7 with sigma of 0.02
 C2-C1D
 1.7 with sigma of 0.02
 C1H-C20
 1.7 with sigma of 0.02
 C4-C1F
 1.7 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uiso(H10) = Uiso(C10) = Uiso(O19) = Uiso(O1B) = Uiso(O1A) = Uiso(C13) =
Uiso(H13B) = Uiso(H13A)
Uiso(H15) = Uiso(C15) = Uiso(O1H) = Uiso(O1F) = Uiso(O1G) = Uiso(C16) =
Uiso(H16)
Uiso(H9) = Uiso(C9) = Uiso(O1E) = Uiso(O1C) = Uiso(O1D) = Uiso(H17B) =
Uiso(C17) = Uiso(H17A)
Uiso(H14) = Uiso(C14) = Uiso(O1K) = Uiso(O1I) = Uiso(C1A) = Uiso(O1J) =
Uiso(H1AB) = Uiso(H1AA)
Uiso(H1B) = Uiso(C1B) = Uiso(O1L) = Uiso(O1N) = Uiso(H1CA) = Uiso(C1C) =
Uiso(O1M) = Uiso(H1CB)
Uiso(H1D) = Uiso(C1D) = Uiso(O1O) = Uiso(O1Q) = Uiso(O1P) = Uiso(C1E) =
Uiso(H1EB) = Uiso(H1EA)
Uiso(C1I) = Uiso(H1IB) = Uiso(H1IA) = Uiso(O1V) = Uiso(O1W) = Uiso(O1S) =
Uiso(C1H) = Uiso(H1H)
Uiso(H1F) = Uiso(C1F) = Uiso(O1R) = Uiso(O1U) = Uiso(O1T) = Uiso(C1G) =
Uiso(H1GB) = Uiso(H1GA)
3. Others
 Fixed Sof: O6(0.5) O8(0.5) O10(0.85) O12(0.85) O15(0.85) O16(0.85) O20(0.85)
 C21(0.85) O22(0.85) C27(0.85) C29(0.85) C34(0.85) C41(0.85) O1(0.85) O2(0.85)
 O3(0.85) O4(0.85) C5(0.85) C6(0.85) C7(0.85) C8(0.85) O0AA(0.85) C2(0.85)
 C4(0.85) C0AA(0.85) C1AA(0.85) C11(0.85) C12(0.85) O13(0.85) C19(0.85)
 C1(0.85) C2AA(0.85) C3(0.85) C4AA(0.85) C3AA(0.85) C5AA(0.85) C18(0.85)
 O1AA(0.5) O11(0.5) O6AA(0.25) O8AA(0.25) O5AA(0.25) O9(0.25) O2AA(0.25)
 O3AA(0.25) O4AA(0.25) C20(0.85) O4BA(0.15) O5BA(0.15) O9AA(0.15) O0BA(0.15)
 O1BA(0.15) O14(0.15) O3BA(0.15) O17(0.15) O18(0.15) O8BA(0.25) O6BA(0.25)
 O7BA(0.25) O7AA(0.33333) O9BA(0.15) O0CA(0.15) O57(0.1) O2CA(0.33333)
 O2BA(0.15) O1CA(0.33333) O3CA(0.25) C10(0.1) C13(0.1) H13A(0.1) H13B(0.1)
 H10(0.1) O19(0.1) O1A(0.1) O1B(0.1) C15(0.1) C16(0.1) H16(0.1) H15(0.1)
 O1F(0.1) O1G(0.1) O1H(0.1) C9(0.1) C17(0.1) H17A(0.1) H17B(0.1) H9(0.1)
 O1C(0.1) O1D(0.1) O1E(0.1) C14(0.1) C1A(0.1) H1AA(0.1) H1AB(0.1) H14(0.1)
 O1I(0.1) O1J(0.1) O1K(0.1) C1B(0.1) C1C(0.1) H1CA(0.1) H1CB(0.1) H1B(0.1)
 O1L(0.1) O1M(0.1) O1N(0.1) C1D(0.1) C1E(0.1) H1EA(0.1) H1EB(0.1) H1D(0.1)
 O1O(0.1) O1P(0.1) O1Q(0.1) C1H(0.1) C1I(0.1) H1IA(0.1) H1IB(0.1) H1H(0.1)
 O1S(0.1) O1V(0.1) O1W(0.1) C1F(0.1) C1G(0.1) H1GA(0.1) H1GB(0.1) H1F(0.1)
 O1R(0.1) O1T(0.1) O1U(0.1)
4.a Free rotating group:
 C10(C13,H13A,H13B,H10,O19,O1A,O1B), C15(C16,H16,H15,O1F,O1G,O1H), C9(C17,H17A,
 H17B,H9,O1C,O1D,O1E), C14(C1A,H1AA,H1AB,H14,O1I,O1J,O1K), C1B(C1C,H1CA,H1CB,
 H1B,O1L,O1M,O1N), C1D(C1E,H1EA,H1EB,H1D,O1O,O1P,O1Q), C1H(C1I,H1IA,H1IB,H1H,
 O1S,O1V,O1W), C1F(C1G,H1GA,H1GB,H1F,O1R,O1T,O1U)
;
_olex2_submission_special_instructions 'No special instructions were received'