Chiral and robust Zr(IV)-based metal-organic frameworks built from spiro skeletons.
Gong, Wei; Liu, Yan; Cui, Yong; Faraday discussions 231 (2021) 168–180; doi:10.1039/d1fd00014d

data_1562008
_publ_section_title
;
 Chiral and robust Zr(IV)-based metal-organic frameworks built from spiro
 skeletons.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              168
_journal_page_last               180
_journal_paper_doi               10.1039/d1fd00014d
_journal_volume                  231
_journal_year                    2021
_chemical_formula_moiety         'C61 H42 O17 Zr3'
_chemical_formula_sum            'C61 H42 O17 Zr3'
_chemical_formula_weight         1320.60
_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_Hall           'I 4bw 2bw'
_space_group_name_H-M_alt        'I 41 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2021-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   42.697(6)
_cell_length_b                   42.697(6)
_cell_length_c                   37.907(8)
_cell_measurement_reflns_used    426047
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.476
_cell_measurement_theta_min      0.674
_cell_volume                     69106(2)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            32461
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.476
_diffrn_reflns_theta_min         0.674
_exptl_absorpt_coefficient_mu    0.201
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.508
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             10624
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         31970
_refine_ls_number_restraints     561
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1074P)^2^+9.9913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                16168
_reflns_number_total             31970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1fd00014d5.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1562006--1562010.cif.'
_cod_original_cell_volume        69106(24)
_cod_database_code               1562008
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(5)
 0.47(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups, All Zr(O,O) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 Zr2-O4
 2.15 with sigma of 0.02
 C57-O7
 1.36 with sigma of 0.02
 C57-O8
 1.25 with sigma of 0.02
 C27-C57
 1.52 with sigma of 0.02
 C37-C32
 1.52 with sigma of 0.02
 C56-C42
 1.52 with sigma of 0.02
 C41-C54
 1.52 with sigma of 0.02
 C55-C56
 1.52 with sigma of 0.02
 C11-C6
 1.52 with sigma of 0.02
 O3-C14
 1.36 with sigma of 0.02
 C13-C59
 1.52 with sigma of 0.02
 C59-C60
 1.52 with sigma of 0.02
 C12-C61
 1.52 with sigma of 0.02
 C60-C61
 1.52 with sigma of 0.02
 O5-C58
 1.25 with sigma of 0.01
 C58-O4
 1.25 with sigma of 0.01
 C43-C39
 1.52 with sigma of 0.02
 C53-C48
 1.52 with sigma of 0.02
 C53-O16
 1.25 with sigma of 0.02
 C53-O17
 1.25 with sigma of 0.02
 O1-C62
 1.25 with sigma of 0.02
 C48-C53
 1.52 with sigma of 0.02
 C58-C22
 1.52 with sigma of 0.02
 C15-C17
 1.52 with sigma of 0.02
 O4-O5
 2.35 with sigma of 0.02
 O14-H14A = O14-H14B = O6-H6A = O6-H6B = O12-H12A = O12-H12B
 0.82 with sigma of 0.01
 C60-C60_$1
 2.56 with sigma of 0.02
 C62-O2
 1.27 with sigma of 0.01
 C62-O1
 1.27 with sigma of 0.01
 C58-C23
 2.48 with sigma of 0.02
 C21-C58
 2.48 with sigma of 0.02
 O16-O17
 2.35 with sigma of 0.02
 H14A-H14B = H6A-H6B = H12A-H12B
 1.39 with sigma of 0.01
 O1-O2
 2.36 with sigma of 0.02
 O3-C13
 2.48 with sigma of 0.04
 O8-C27 \\sim C27-O7
 with sigma of 0.02
 C36-C57 \\sim C57-C28
 with sigma of 0.02
 C12-C6 \\sim C6-C16
 with sigma of 0.02
 C47-C53 \\sim C53-C49
 with sigma of 0.02
 C23-C58 \\sim C58-C21
 with sigma of 0.02
 C14-C18 \\sim C18-C16
 with sigma of 0.02
 C38-C43 \\sim C43-C40
 with sigma of 0.02
 C16-C17 \\sim C17-C14
 with sigma of 0.02
 C26-C15 \\sim C15-C18
 with sigma of 0.02
 O4-C22 \\sim O5-C22
 with sigma of 0.02
4. Restrained planarity
 O8, C57, O7, C27, C36, C28
 with sigma of 0.1
 C6, C11, C16, C12
 with sigma of 0.1
 C49, C48, C47, C53
 with sigma of 0.1
 C48, O17, C53, O16
 with sigma of 0.1
 C43, C39, C40, C38
 with sigma of 0.1
 C24, C19, C25, C26, C17
 with sigma of 0.1
 C58, C22, C23, C21
 with sigma of 0.1
 O5, O4, C58, C22
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim O9 \\sim O10 \\sim O15 \\sim O7 \\sim O13 \\sim O1 \\sim O2
\\sim O8 \\sim O3 \\sim O14 \\sim O6 \\sim O17 \\sim O16 \\sim O11 \\sim O12
\\sim C55 \\sim C56 \\sim C54 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C57 \\sim C62 \\sim C9 \\sim C10 \\sim C1 \\sim C2 \\sim C3
\\sim C8 \\sim C7 \\sim C6 \\sim C5 \\sim C4 \\sim C36 \\sim C27 \\sim C28
\\sim C29 \\sim C30 \\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C31 \\sim C12
\\sim C11 \\sim C16 \\sim C15 \\sim C14 \\sim C13 \\sim C51 \\sim C52 \\sim C43
\\sim C44 \\sim C45 \\sim C50 \\sim C49 \\sim C48 \\sim C47 \\sim C46 \\sim C59
\\sim C58 \\sim C60 \\sim C61 \\sim C53 \\sim C23 \\sim C22 \\sim C21 \\sim C20
\\sim C19 \\sim C24 \\sim C25 \\sim C26 \\sim C17 \\sim C18: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B), C60(H60A,H60B), C61(H61A,H61B)
6.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C9(H9), C10(H10), C2(H2), C7(H7), C5(H5), C4(H4), C36(H36),
 C28(H28), C29(H29), C34(H34), C33(H33), C31(H31), C16(H16), C51(H51), C52(H52),
  C44(H44), C49(H49), C47(H47), C46(H46), C23(H23), C21(H21), C20(H20),
 C25(H25), C26(H26), C18(H18)
6.c Fitted hexagon refined as free rotating group:
 C37(C38,C39,C40,C41,C42), C12(C11,C16,C15,C14,C13)
6.d X=CH2 refined with riding coordinates:
 O14(H14A,H14B), O6(H6A,H6B), O12(H12A,H12B)
6.e Naphthalene refined as free rotating group:
 C9(C10,C1,C2,C3,C8,C7,C6,C5,C4), C36(C27,C28,C29,C30,C35,C34,C33,C32,C31),
 C51(C52,C43,C44,C45,C50,C49,C48,C47,C46), C23(C22,C21,C20,C19,C24,C25,C26,C17,
 C18)
6.f Idealised tetrahedral OH refined as rotating group:
 O15(H15), O3(H3)
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_shelx_res_checksum              17877
_shelx_fab_checksum              70852
_olex2_submission_special_instructions 'No special instructions were received'