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_1562007
_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_absolute_configuration rm
_chemical_formula_moiety         'C135 H78 O40 Zr6'
_chemical_formula_sum            'C135 H78 O40 Zr6'
_chemical_formula_weight         2887.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc251k4y
_audit_creation_date             2020-10-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-09 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            8
_cell_length_a                   25.626(5)
_cell_length_b                   30.235(6)
_cell_length_c                   61.873(12)
_cell_measurement_reflns_used    254943
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.991
_cell_measurement_theta_min      1.092
_cell_volume                     47939(16)
_computing_cell_refinement       hkl3000
_computing_data_collection       BL17B
_computing_data_reduction        hkl3000
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.116
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_number            22879
_diffrn_reflns_point_group_measured_fraction_full 0.505
_diffrn_reflns_point_group_measured_fraction_max 0.486
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_min         1.092
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.800
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             11584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1289
_refine_ls_number_reflns         22879
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0871P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                15298
_reflns_number_total             22879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1fd00014d4.cif
_cod_data_source_block           Spiro-OH
_cod_depositor_comments
'Adding full bibliography for 1562006--1562010.cif.'
_cod_original_cell_volume        47939(17)
_cod_database_code               1562007
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.930
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C787-C03X
 1.52 with sigma of 0.02
 C922-C409
 1.52 with sigma of 0.02
 C03Y-C03J
 1.52 with sigma of 0.02
 C111-C040
 1.5 with sigma of 0.02
 O271-C787
 1.27 with sigma of 0.02
 O00H-C787
 1.27 with sigma of 0.02
 C900-O447
 1.36 with sigma of 0.02
 C850-C232
 1.52 with sigma of 0.02
 O011-C850
 1.27 with sigma of 0.02
 C280-C04C
 1.55 with sigma of 0.02
 C215-C04C
 1.55 with sigma of 0.02
 C04O-C04C
 1.52 with sigma of 0.02
 C229-C122
 1.52 with sigma of 0.02
 C280-C229
 1.55 with sigma of 0.02
 C405-C04C
 1.52 with sigma of 0.02
 C409-C215
 1.55 with sigma of 0.02
 O325-C850
 1.27 with sigma of 0.02
 O013-C042
 1.27 with sigma of 0.02
 O019-C042
 1.27 with sigma of 0.02
 C662-C546
 1.5 with sigma of 0.02
 C809-C539
 1.5 with sigma of 0.01
 C248-C042
 1.5 with sigma of 0.01
 C049-C048
 1.5 with sigma of 0.01
 O00H-O271
 2.36 with sigma of 0.04
 C656-C567
 2.41 with sigma of 0.02
 O325-O011
 2.25 with sigma of 0.04
 O011-O325
 2.25 with sigma of 0.04
 C04O-C280
 2.36 with sigma of 0.04
 C122-C280
 2.36 with sigma of 0.04
 C405-C215
 2.36 with sigma of 0.04
 C922-C215
 2.36 with sigma of 0.04
 C04O-C215
 2.36 with sigma of 0.02
 H71-H615
 2.6 with sigma of 0.02
 C615-C809 \\sim C809-C104
 with sigma of 0.02
 C71-C539 \\sim C539-C922
 with sigma of 0.02
 C45-C787 \\sim C787-C04J
 with sigma of 0.02
 C583-C042 \\sim C042-C04N
 with sigma of 0.02
 C656-C546 \\sim C546-C567
 with sigma of 0.02
 C777-C850 \\sim C850-C479
 with sigma of 0.02
 C104-C809 \\sim C809-C615
 with sigma of 0.02
 O011-C232 \\sim C232-O325
 with sigma of 0.02
 C405-O447 \\sim O447-C546
 with sigma of 0.02
 C900-C662 \\sim C662-C71
 with sigma of 0.01
 C922-C539 \\sim C539-C71
 with sigma of 0.02
 O011-C850 \\sim C850-O325
 with sigma of 0.01
3. Restrained planarity
 C04O, C35, C049, C111, C03W, C122, C229, C04C
 with sigma of 0.1
 C922, C405, C900, C04C, C409
 with sigma of 0.1
 C04N, C248, C583, C042
 with sigma of 0.1
 C809, C539, C104, C615, C583, C248, C04N, C042, O019, O013
 with sigma of 0.01
 C900, C546, C71, C662
 with sigma of 0.01
 C546, C662, C656, C567, C777, C479, C232, O011, O325, C850
 with sigma of 0.01
 C049, C35, O36, C04O
 with sigma of 0.01
 C615, C539, C104, C809, C04N, C248, C583
 with sigma of 0.001
 C546, C662, C567, C479, C656
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C539) = Uanis(C615) = Uanis(C583) = Uanis(C248) = Uanis(C04N) =
Uanis(C104) = Uanis(O013) = Uanis(C042) = Uanis(O019)
Uanis(O271) = Uanis(O00H)
Uanis(O325) = Uanis(O011) = Uanis(C850)
Uanis(C232) = Uanis(C662)
Uanis(C71) = Uanis(C809)
Uanis(C656) = Uanis(C777) = Uanis(C232) = Uanis(C479) = Uanis(C567) =
Uanis(C662)
Uanis(C04C) = Uanis(C04O)
Uanis(C922) = Uanis(C900)
Uanis(C546) = Uanis(C900)
Uanis(C922) = Uanis(C405)
5. Rigid body (RIGU) restrains
 O011, C850, O325, C232, C777, C656, C662, C567, C479
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C787, O00H, O271
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C900, C546, C71, C809, C922, C405
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C900, C546, C662
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C546, C567, C656, C850, C71, C662, C479, C232, C777, C900, C405, C922, C809
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C04O, C04C, C280, C229, C122
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C01O(H01A,H01B), C023(H02B,H02D), C02I(H02E,H02F), C02L(H02G,H02H), C02M(H02I,
 H02J), C039(H03B,H03C), C03F(H03F,H03G), C03N(H03J,H03K), C215(H21A,H21B),
 C409(H40A,H40B), C229(H22A,H22B), C280(H28A,H28B)
6.b Aromatic/amide H refined with riding coordinates:
 C02O(H02O), C02Z(H02Z), C02U(H02U), C028(H028), C037(H037), C02Q(H02Q),
 C03E(H03E), C02A(H02A), C033(H033), C03I(H03I), C03D(H03D), C02N(H02N),
 C036(H036), C01P(H01P), C01R(H01R), C01X(H01X), C02C(H02C), C02Y(H02Y),
 C02W(H02W), C01K(H01K), C02V(H02V), C03O(H03O), C025(H025), C01M(H01M),
 C030(H030), C02K(H02K), C026(H026), C03A(H03A), C03H(H03H), C038(H038),
 C02R(H02R), C034(H034), C03L(H03L), C03M(H03M), C043(H043), C04E(H04E),
 C196(H196), C04J(H04J), C45(H45), C101(H101), C03R(H03R), C041(H041),
 C044(H044), C046(H046), C03W(H03W), C04N(H04N), C583(H583), C615(H615),
 C104(H104), C71(H71), C567(H567), C479(H479), C777(H777), C656(H656)
6.c Fitted hexagon refined as free rotating group:
 C012(C02O,C022,C02D,C01Y,C01W), C018(C02Z,C02U,C01E,C028,C037), C01A(C01L,
 C01T,C02Q,C03B,C02H), C01D(C01V,C01G,C02T,C027,C03E), C01H(C02A,C033,C031,C03I,
 C03D), C01I(C02N,C036,C020,C01P,C01R), C01J(C01X,C02C,C02E,C02Y,C02W),
 C01K(C01S,C02V,C03O,C01N,C025), C01M(C029,C030,C02K,C01U,C026), C01Z(C03A,C03H,
 C035,C038,C02R), C02G(C03C,C02X,C02P,C032,C034), C03L(C03U,C03M,C043,C048,
 C04E), C03P(C196,C04J,C03X,C45,C101), C03R(C041,C040,C044,C046,C03Y),
 C03W(C111,C122,C04O,C35,C049), C04N(C248,C583,C615,C539,C104), C405(C922,C809,
 C71,C546,C900), C567(C479,C232,C777,C656,C662)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94968
_shelx_fab_checksum              91137
_olex2_submission_special_instructions 'No special instructions were received'