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_1562006
_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         'C283 H244 N2 O98 Zr12, 36[C3H7NO]'
_chemical_formula_sum            'C195.5 H248 N19 O67 Zr6'
_chemical_formula_weight         4483.43
_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.cc23znh8
_audit_creation_date             2020-10-06
_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                   25.1903(10)
_cell_length_b                   29.0888(12)
_cell_length_c                   64.585(3)
_cell_measurement_reflns_used    9317
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.24
_cell_measurement_theta_min      2.18
_cell_volume                     47325(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            217968
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        23.258
_diffrn_reflns_theta_max         23.258
_diffrn_reflns_theta_min         1.400
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.4451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       triangle
_exptl_crystal_F_000             18640
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 13740 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.531(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1638
_refine_ls_number_reflns         33816
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.884
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                31375
_reflns_number_total             33816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1fd00014d3.cif
_cod_data_source_block           Spiro-CE-1
_cod_depositor_comments
'Adding full bibliography for 1562006--1562010.cif.'
_cod_original_formula_sum        'C195.50 H248 N19 O67 Zr6'
_cod_database_code               1562006
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.921
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C100-C101
 1.55 with sigma of 0.02
 C101-O44
 1.42 with sigma of 0.02
 C24-O74
 1.42 with sigma of 0.02
 O74-C108
 1.42 with sigma of 0.02
 C108-C109
 1.55 with sigma of 0.02
 O47-C107
 1.55 with sigma of 0.02
 O46-C105
 1.55 with sigma of 0.02
 C105-C104
 1.55 with sigma of 0.02
 O44-C101
 1.42 with sigma of 0.02
 C101-C100
 1.55 with sigma of 0.02
 C100-O43
 1.42 with sigma of 0.02
 O42-C64
 1.42 with sigma of 0.02
 C64-O42
 1.42 with sigma of 0.02
 O42-C125
 1.42 with sigma of 0.02
 C125-C126
 1.55 with sigma of 0.02
 C126-O41
 1.42 with sigma of 0.02
 O41-C127
 1.42 with sigma of 0.02
 C128-C127
 1.55 with sigma of 0.02
 C128-O40
 1.42 with sigma of 0.02
 O40-C129
 1.42 with sigma of 0.02
 C84-O32
 1.42 with sigma of 0.02
 O32-C94
 1.42 with sigma of 0.02
 C94-C95
 1.55 with sigma of 0.02
 C97-O34
 1.42 with sigma of 0.02
 C118-O35
 1.42 with sigma of 0.02
 C118-C119
 1.55 with sigma of 0.02
 N1-C92
 1.45 with sigma of 0.02
 N1-C93
 1.45 with sigma of 0.02
 N1-C91
 1.45 with sigma of 0.02
 C91-O14
 1.22 with sigma of 0.02
 C109-O47
 1.42 with sigma of 0.02
 C107-O47
 1.42 with sigma of 0.02
 C107-C106
 1.55 with sigma of 0.02
 C106-O46
 1.42 with sigma of 0.02
 C105-O46
 1.42 with sigma of 0.02
 C104-C105
 1.55 with sigma of 0.02
 C104-O45
 1.42 with sigma of 0.02
 O45-C103
 1.42 with sigma of 0.02
 O44-C102
 1.42 with sigma of 0.02
 C103-C102
 1.55 with sigma of 0.02
 O33-C95
 1.45 with sigma of 0.02
 C97-C96
 1.55 with sigma of 0.02
 C95-O33
 1.42 with sigma of 0.02
 O33-C96
 1.42 with sigma of 0.02
 C98-O34
 1.42 with sigma of 0.02
 C121-C120
 1.55 with sigma of 0.02
 O37-C122
 1.42 with sigma of 0.02
 O37-C121
 1.42 with sigma of 0.02
 O36-C120
 1.42 with sigma of 0.02
 C98-C98_$2
 1.55 with sigma of 0.01
 C129-C129_$3
 1.55 with sigma of 0.01
 C122-C122_$1
 1.55 with sigma of 0.01
 C28-C140
 1.5 with sigma of 0.01
 C92-C93
 2.35 with sigma of 0.04
 C104-O46
 2.36 with sigma of 0.04
 C96-C95
 2.36 with sigma of 0.04
 O33-C97
 2.36 with sigma of 0.04
 C96-O34
 2.36 with sigma of 0.04
 C84-C94
 2.36 with sigma of 0.04
 C95-C96
 2.36 with sigma of 0.04
 C97-C98
 2.36 with sigma of 0.02
 C119-C120
 2.48 with sigma of 0.04
 O36-C121
 2.48 with sigma of 0.04
 C121-C122
 2.48 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C122, O37, C121, C120, O36, C119
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C95, O33, C96, C97, O34, C98
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C133(H13A,H13B), C113(H11A,H11B), C112(H11C,H11D), C132(H13C,H13D), C2AA(H2AA,
 H2AB), C111(H11E,H11F), C139(H13E,H13F), C100(H10A,H10B), C101(H10C,H10D),
 C110(H11G,H11H), C117(H11I,H11J), C288(H28A,H28B), C125(H12A,H12B), C108(H10E,
 H10F), C109(H10G,H10H), C127(H12C,H12D), C105(H10I,H10J), C104(H10K,H10L),
 C106(H10M,H10N), C107(H10O,H10P), C128(H12E,H12F), C129(H12G,H12H), C119(H11K,
 H11L), C94(H94A,H94B), C118(H11M,H11N), C95(H95A,H95B), C97(H97A,H97B),
 C96(H96A,H96B), C103(H10Q,H10R), C102(H10S,H10T), C98(H98A,H98B), C120(H12I,
 H12J), C121(H12K,H12L), C122(H12M,H12N)
4.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C39(H39), C41(H41), C42(H42), C3(H3), C2(H2), C6(H6), C5(H5),
 C54(H54), C18(H18), C17(H17), C15(H15), C14(H14), C53(H53), C60(H60), C59(H59),
  C57(H57), C56(H56), C62(H62), C44(H44), C36(H36), C12(H12), C68(H68),
 C69(H69), C71(H71), C72(H72), C35(H35), C89(H89), C90(H90), C86(H86), C87(H87),
  C78(H78), C77(H77), C75(H75), C74(H74), C22(H22), C33(H33), C126(H126),
 C32(H32), C29(H29), C27(H27), C26(H26), C30(H30), C51(H51), C50(H50), C80(H80),
  C135(H135), C91(H91)
4.c Fitted hexagon refined as free rotating group:
 C38(C39,C40,C41,C42,C37), C4(C3,C2,C1,C6,C5), C18(C17,C16,C15,C14,C13),
 C55(C60,C59,C58,C57,C56), C64(C65,C66,C61,C62,C63), C44(C43,C48,C47,C46,C45),
 C9(C8,C7,C12,C11,C10), C68(C69,C70,C71,C72,C67), C88(C89,C90,C85,C86,C87),
 C73(C78,C77,C76,C75,C74), C24(C23,C22,C21,C20,C19), C29(C28,C27,C26,C25,C30)
4.d Idealised Me refined as rotating group:
 C93(H93A,H93B,H93C), C92(H92A,H92B,H92C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28680
_shelx_fab_checksum              47857
_olex2_submission_special_instructions 'No special instructions were received'