A meta-xylenediamide macrocycle containing rotaxane anion host system constructed by a new synthetic clipping methodology
Evans, Nicholas H.; Serpell, Christopher J.; Beer, Paul D.; New Journal of Chemistry 35 (2011) 2047–; doi:10.1039/c1nj20109c

data_7052708
_publ_section_title
;
 A meta-xylenediamide macrocycle containing rotaxane anion host system
 constructed by a new synthetic clipping methodology
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2047
_journal_paper_doi               10.1039/c1nj20109c
_journal_volume                  35
_journal_year                    2011
_chemical_formula_moiety
;
C74 H78 N3 O2, C32 H38 N2 O9, 0.48(C H Cl3), Cl
;
_chemical_formula_sum            'C106.48 H116.48 Cl2.45 N5 O11'
_chemical_formula_weight         1729.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-11-25
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                90
_cell_angle_beta                 97.333(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.498(6)
_cell_length_b                   29.702(16)
_cell_length_c                   31.391(17)
_cell_measurement_reflns_used    29790
_cell_measurement_temperature    293
_cell_measurement_theta_max      59
_cell_measurement_theta_min      2
_cell_volume                     10633(10)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2009)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2009)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2009)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Si(1 1 1) double-crystal monochromator'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.162
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23420
_diffrn_reflns_theta_full        51.937
_diffrn_reflns_theta_max         89.546
_diffrn_reflns_theta_min         2.056
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 1997--2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3680.370
_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.027
_platon_squeeze_details
;
The PLATON/SQUEEZE routine was used to model the disordered solvent
cavity because there was no discernible structure in the Fourier
difference map within this volume. It is therefore very difficult to
know what proportion of the two solvents used in crystallisation
occupy the cavity (even considering the electron count derived using
SQUEEZE), and therefore it was deemed inappropriate to include such
speculative information in the data reported in Supplementary Table 1.
;
_refine_diff_density_max         1.20
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1455
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         11241
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.2083
_refine_ls_R_factor_gt           0.1371
_refine_ls_shift/su_max          0.0002792
_refine_ls_shift/su_mean         0.0000188
_refine_ls_structure_factor_coef F
_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:
-0.120 -1.84 -1.03 -0.959 -0.189
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0895
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0616
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              38
_reflns_limit_k_min              0
_reflns_limit_l_max              40
_reflns_limit_l_min              0
_reflns_number_gt                11241
_reflns_number_total             23420
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.07
_oxford_diffrn_Wilson_scale      117.97
_oxford_refine_ls_r_factor_ref   0.1371
_oxford_refine_ls_scale          0.1722(3)
_oxford_reflns_number_all        23332
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 009CJS10
_cod_data_source_file            c1nj20109c.txt
_cod_data_source_block           5Cl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        10630(10)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7052708