Polyyne Rotaxanes: Stabilization by Encapsulation.
Movsisyan, Levon D.; Franz, Michael; Hampel, Frank; Thompson, Amber L.; Tykwinski, Rik R.; Anderson, Harry L.; Journal of the American Chemical Society 138 (2016) 1366–1376; doi:10.1021/jacs.5b12049

data_4129937
_publ_section_title
;
 Polyyne Rotaxanes: Stabilization by Encapsulation.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1366
_journal_page_last               1376
_journal_paper_doi               10.1021/jacs.5b12049
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C98 H126, C36 H30 N2 O4, 0.15(C H2 Cl2), 0.85(C H4 O)'
_chemical_formula_sum            'C135 H159.7 Cl0.3 N2 O4.85'
_chemical_formula_weight         1898.70
_chemical_melting_point          ?
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2015-05-28
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 94.4528(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.5428(2)
_cell_length_b                   10.7047(1)
_cell_length_c                   24.0361(2)
_cell_measurement_reflns_used    35017
_cell_measurement_temperature    100
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     5782.74(9)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            98157
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         29.350
_diffrn_reflns_theta_min         1.647
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            clear_pale_yellow
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             2055.181
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.66
_refine_ls_abs_structure_details 'Flack (1983), 14336 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.1(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9750
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1307
_refine_ls_number_reflns         16873
_refine_ls_number_restraints     253
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.0011687
_refine_ls_shift/su_mean         0.0000413
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.329E+04 0.548E+04 0.342E+04 0.150E+04 373. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1727
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1710
_reflns_limit_h_max              31
_reflns_limit_h_min              -31
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                15410
_reflns_number_total             16938
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.43
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.0724
_oxford_refine_ls_scale          5.36(7)
_oxford_reflns_number_all        16886
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title DIA0233
_cod_data_source_file            ja5b12049_si_002.cif
_cod_data_source_block           2c-M2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5782.74(5)
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C135 H159.70 Cl0.30 N2 O4.85'
_cod_database_code               4129937