Redox-Responsive Host-Guest Chemistry of a Flexible Cage with Naphthalene Walls.
Jia, Fei; Schröder, Hendrik V; Yang, Liu-Pan; von Essen, Carolina; Sobottka, Sebastian; Sarkar, Biprajit; Rissanen, Kari; Jiang, Wei; Schalley, Christoph A.; Journal of the American Chemical Society 142 (2020) 3306–3310; doi:10.1021/jacs.9b11685

data_4134159
_publ_section_title
;
 Redox-Responsive Host-Guest Chemistry of a Flexible Cage with Naphthalene
 Walls.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3306
_journal_page_last               3310
_journal_paper_doi               10.1021/jacs.9b11685
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         '2(F6 P), C90 H119 O12, C12 H14 N2'
_chemical_formula_sum            'C102 H133 F12 N2 O12 P2'
_chemical_formula_weight         1869.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.43(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.574(5)
_cell_length_b                   27.719(6)
_cell_length_c                   29.313(6)
_cell_measurement_reflns_used    20026
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_volume                     19714(8)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      153(1)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Apex II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            49913
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.846
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0781 before and 0.0691 after correction. The Ratio of minimum to maximum transmission is 0.9017. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             7944
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1185
_refine_ls_number_reflns         15796
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+82.7095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.2076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9367
_reflns_number_total             15796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11685_si_002.cif
_cod_data_source_block           MV_NC
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_cell_measurement_temperature' value '153(2' was changed
to '153(2)' -- precision was estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 4134159.cif.
;
_cod_original_cell_volume        19713(8)
_cod_database_code               4134159
_shelx_shelxl_version_number     2017/1
_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
 C03J-C03H
 1.54 with sigma of 0.02
 C03D-C03B
 1.54 with sigma of 0.005
 C039-C03G
 1.54 with sigma of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C00Y(H00A,H00B), C012(H01A,H01B), C014(H01C,H01D), C01C(H01E,H01F), C01E(H01G,
 H01H), C01G(H01J,H01K), C01L(H01N,H01O), C01M(H01P,H01Q), C01N(H01R,H01S),
 C01O(H01T,H01U), C01P(H01V,H01W), C01Q(H01X,H01Y), C01R(H01Z,H), C023(H02A,
 H02B), C02C(H02C,H02D), C02G(H02J,H02K), C02H(H02L,H02M), C02I(H02N,H02O),
 C02K(H02P,H02Q), C02L(H02R,H02S), C02T(H02X,H02Y), C02U(H02Z,HC), C02Y(H1AA,
 HH), C033(H03G,H03H), C035(H03L,H03M), C036(H03N,H03O), C037(H03P,H03Q),
 C039(H03R,H03S), C03A(H03T,H03U), C03D(H03Z,HM), C03F(H3AA,HN), C03G(H4AA,HO),
 C03H(H5AA,HP), C03I(H6AA,HQ), C03J(H7AA,HR)
3.b Aromatic/amide H refined with riding coordinates:
 C01F(H01I), C01H(H01L), C01J(H01M), C01V(H01), C01Z(H1BA), C021(H021),
 C022(H022), C024(H024), C025(H025), C027(H027), C029(H029), C02A(H2BA),
 C02B(H3BA), C02D(H02E), C02E(H02F), C02M(H02T), C02N(H4BA), C02Q(H6BA),
 C02W(H02), C031(H031), C03E(H03)
3.c Idealised Me refined as rotating group:
 C02F(H02G,H02H,H02I), C02P(H5BA,HA,HB), C02R(H02U,H02V,H02W), C02V(H7BA,HD,
 HE), C02X(H0AA,HF,HG), C02Z(H2AA,HI,HJ), C030(H03A,H03B,H03C), C032(H03D,H03E,
 H03F), C034(H03I,H03J,H03K), C03B(H03V,H03W,H03X), C03C(H03Y,HK,HL), C03K(H8AA,
 HS,HT), C03L(H9AA,HU,HV), C03M(H0BA,HW,HX)
;
_shelx_res_checksum              38087
_shelx_hkl_checksum              75529
_olex2_submission_special_instructions 'No special instructions were received'