Cooperative Reactivity in an Extended-Viologen-Based Cyclophane.
Dale, Edward J.; Ferris, Daniel P.; Vermeulen, Nicolaas A.; Henkelis, James J.; Popovs, Ilja; Juríček, Michal; Barnes, Jonathan C.; Schneebeli, Severin T.; Stoddart, J. Fraser; Journal of the American Chemical Society 138 (2016) 3667–3670; doi:10.1021/jacs.6b01368

data_4130228
_publ_section_title
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 Cooperative Reactivity in an Extended-Viologen-Based Cyclophane.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3667
_journal_page_last               3670
_journal_paper_doi               10.1021/jacs.6b01368
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C40 H32 N4, 4(F6 P), 0.5(C4 H6 N2)'
_chemical_formula_sum            'C42 H35 F24 N5 P4'
_chemical_formula_weight         1189.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2b 2b'
_space_group_name_H-M_alt        'I c m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-28
_audit_creation_method
;
Olex2 1.2
(compiled Jan 19 2015 12:28:14 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.465(2)
_cell_length_b                   22.063(4)
_cell_length_c                   23.253(4)
_cell_measurement_reflns_used    7954
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.200
_cell_measurement_theta_min      3.802
_cell_volume                     5881.9(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.97
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  prospector
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12875
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        65.238
_diffrn_reflns_theta_max         65.238
_diffrn_reflns_theta_min         3.802
_exptl_absorpt_coefficient_mu    2.185
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0628 before and 0.0395 after correction.
The Ratio of minimum to maximum transmission is 0.8344.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2565
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0910P)^2^+13.4247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2429
_reflns_number_total             2565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b01368_si_005.cif
_cod_data_source_block           cu_cx0456_0m
_cod_original_cell_volume        5882.0(19)
_cod_database_code               4130228
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.544
_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. Uiso/Uaniso restraints and constraints
Uanis(F5A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(F6A)=1-FVAR(1)
 Sof(F6)=FVAR(1)
 Sof(F3A)=1-FVAR(2)
 Sof(F3)=FVAR(2)
 Sof(F4A)=1-FVAR(3)
 Sof(F4)=FVAR(3)
 Sof(F5A)=1-FVAR(4)
 Sof(F5)=FVAR(4)
 Fixed Sof: N2(0.25) C11(0.25) C12(0.25) H12A(0.25) H12B(0.25) H12C(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C9(H9), C10(H10)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_smtbx_masks_special_details
;
Total solvent accessible volume / cell = 1095.4 Ang^3 [18.6%]
Total electron count / cell = 183.8
;
_shelx_res_checksum              38667
_shelx_hkl_checksum              64241
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'