3D vs. turbostratic: controlling metal–organic framework dimensionality via N-heterocyclic carbene chemistry
Kochetygov, Ilia; Justin, Anita; Asgari, Mehrdad; Yang, Shuliang; Karve, Vikram; Schertenleib, Till; Stoian, Dragos; Oveisi, Emad; Mensi, Mounir; Queen, Wendy L.; Chemical Science  (2022) –; doi:10.1039/D2SC01041K

data_1566994
_publ_section_title
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 3D vs. turbostratic: controlling metal--organic framework dimensionality
 via N-heterocyclic carbene chemistry
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01041K
_journal_year                    2022
_chemical_formula_moiety         '0.08(C204 H156 Cu12 N24 O48), B F4'
_chemical_formula_sum            'C17 H13 B Cu F4 N2 O4'
_chemical_formula_weight         459.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2021-12-14 deposited with the CCDC.	2022-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.450(6)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.932(3)
_cell_length_b                   31.562(5)
_cell_length_c                   14.861(3)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.424
_cell_measurement_theta_min      0.001
_cell_volume                     6928(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  Bruker_D8_Venture
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1906
_diffrn_reflns_av_unetI/netI     0.1227
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            79663
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        23.424
_diffrn_reflns_theta_max         23.424
_diffrn_reflns_theta_min         0.645
_exptl_absorpt_coefficient_mu    0.999
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       needle
_exptl_crystal_F_000             2772
_refine_diff_density_max         1.862
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.269
_refine_ls_extinction_coef       0.0014(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.488
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9973
_refine_ls_number_restraints     459
_refine_ls_restrained_S_all      1.485
_refine_ls_R_factor_all          0.2099
_refine_ls_R_factor_gt           0.1261
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3637
_refine_ls_wR_factor_ref         0.4251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5601
_reflns_number_total             9973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01041k2.cif
_cod_data_source_block           cu_sp5_bf4_a_etoh_0m_sq
_cod_database_code               1566994
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.9327(17)
 0.0673(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Rigid bond restraints
 B02B, F008, F00M, F00O, F017
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O007, O00A, C01C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cu01, Cu03
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O005, O00A, O00D, Cu02
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O007 \\sim O00A \\sim C01C: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C01I \\sim C01G: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cu02 \\sim O005: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
O00T \\sim O00F \\sim Cu03: within 2.6A with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(Cu01) \\sim Ueq, Uanis(Cu03) \\sim Ueq, Uanis(Cu02) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.001
Uanis(C00Q) = Uanis(C01A) = Uanis(C00Y) = Uanis(C015) = Uanis(C01B) =
Uanis(C022)
Uanis(C018) = Uanis(C026)
Uanis(O006) = Uanis(O00P) = Uanis(C01O)
Uanis(C026) = Uanis(C018) = Uanis(N00E) = Uanis(N00L) = Uanis(C00W)
Uanis(O007) = Uanis(O00A) = Uanis(C01C) = Uanis(C01W) = Uanis(C01E) =
Uanis(C01P) = Uanis(C014) = Uanis(C01K) = Uanis(C021)
Uanis(O005) = Uanis(O00D) = Uanis(C01Y)
Uanis(C011) = Uanis(C2) = Uanis(C1) = Uanis(C01S) = Uanis(C00U) = Uanis(C01H) =
Uanis(C00S) = Uanis(O00C) = Uanis(O00F)
Uanis(O009) = Uanis(O00H) = Uanis(C01V)
Uanis(C010) = Uanis(C01I) = Uanis(C01M) = Uanis(C01R) = Uanis(C01Z) =
Uanis(C02A)
Uanis(N00J) = Uanis(C01F) = Uanis(C01L) = Uanis(N00K) = Uanis(C00Z)
Uanis(N00L) = Uanis(C00W) = Uanis(N00E) = Uanis(C018) = Uanis(C026)
Uanis(C01X) = Uanis(C025) = Uanis(C013) = Uanis(C00X) = Uanis(C020) =
Uanis(C029)
Uanis(Cu01) = Uanis(Cu03)
Uanis(Cu02) = Uanis(Cu03)
5. Rigid body (RIGU) restrains
 C00U, C011, C1, C01H, C01S, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N00B, N00N, C01J, C01T, C024
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00Q, C00Y, C015, C01A, C01B, C022
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C010, C01I, C01M, C01R, C01Z, C02A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N00E, N00L, C00W, C018, C026
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00X, C013, C01X, C020, C025, C029
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C014, C01E, C01K, C01P, C01W, C021
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C01F, C01L, N00K, C00Z, N00J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C019, C01N, C01Q, C01U, C023, C028
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O007, O00A, C01C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O005, O00D, C01Y
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O006, O00P, C01O
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O00I, O00T, C01G, O00F, C00S, O00C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O00C, C00S, O00F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, B2, F3, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N00E, C00X
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C010, N00L
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cu02, O005
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Cu03, O00F
 with sigma for 1-2 distances of 0.00001 and sigma for 1-3 distances of 0.00001
6.a Free rotating group:
 B2(F3,F4,F5,F6)
6.b Secondary CH2 refined with riding coordinates:
 C018(H01A,H01B), C01F(H01E,H01F), C01L(H01G,H01I), C01T(H01K,H01L), C024(H02A,
 H02B), C026(H02C,H02D)
6.c Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C00Y(H00Y), C00Z(H00Z), C011(H011), C014(H014), C019(H019),
 C01A(H01C), C01B(H01D), C01H(H01H), C01J(H01J), C01M(H01M), C01N(H01N),
 C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S), C01W(H01W), C01X(H01X),
 C01Z(H01Z), C020(H020), C021(H021), C022(H022), C025(H025), C2(H2), C028(H028),
  C029(H029), C02A(H02E)
;
_shelx_res_checksum              71386
_shelx_fab_checksum              38314
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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