Conformational changes in Cmethyl-resorcinarene pyridine N-oxide inclusion complexes in the solid state
Puttreddy, Rakesh; Beyeh, Ngong Kodiah; Rissanen, Kari; CrystEngComm 18 (2016) 4971–; doi:10.1039/C6CE00240D

data_7224405
_publ_section_title
;
 Conformational changes in Cmethyl-resorcinarene pyridine N-oxide
 inclusion complexes in the solid state
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4971
_journal_paper_doi               10.1039/C6CE00240D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '2(C6 H7 N O2), C32 H32 O8'
_chemical_formula_sum            'C44 H46 N2 O12'
_chemical_formula_weight         794.83
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-28 deposited with the CCDC.
2016-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6411(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6065(3)
_cell_length_b                   14.6623(3)
_cell_length_c                   14.2271(3)
_cell_measurement_reflns_used    9711
_cell_measurement_temperature    123.0
_cell_measurement_theta_max      73.1520
_cell_measurement_theta_min      3.8470
_cell_volume                     3787.27(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000   60.0000 82

  2 omega -117.00   -4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -19.0000 -120.0000 113

  3 omega    2.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676  -99.0000 -180.0000 80

  4 omega   45.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676 -125.0000   90.0000 51

  5 omega   23.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -94.0000  -60.0000 86

  6 omega   33.00  122.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154 -125.0000 -120.0000 89

  7 omega   95.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  125.0000    0.0000 80

  8 omega   79.00  172.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   30.0000 -180.0000 93

  9 omega   30.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -30.0000   30.0000 60

 10 omega   79.00  176.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   30.0000   90.0000 97

 11 omega   31.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -30.0000  -90.0000 60

 12 omega   29.00  138.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -77.0000   30.0000 109

 13 omega -115.00  -13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -57.0000  150.0000 102

 14 omega -118.00   -9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -77.0000   60.0000 109

 15 omega    1.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676  -99.0000  -90.0000 81

 16 omega   73.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   77.0000    0.0000 42

 17 omega   73.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   77.0000 -150.0000 105

 18 omega   77.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   30.0000  -30.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0724644000
_diffrn_orient_matrix_UB_12      0.0532513000
_diffrn_orient_matrix_UB_13      0.0079207000
_diffrn_orient_matrix_UB_21      0.0277059000
_diffrn_orient_matrix_UB_22      -0.0361026000
_diffrn_orient_matrix_UB_23      0.1032738000
_diffrn_orient_matrix_UB_31      0.0345185000
_diffrn_orient_matrix_UB_32      -0.0828924000
_diffrn_orient_matrix_UB_33      -0.0399762000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16391
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         66.744
_diffrn_reflns_theta_min         3.875
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91492
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.1322
_exptl_crystal_size_mid          0.0824
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0432P)^2^+2.5663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3081
_reflns_number_total             3356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00240d2.cif
_cod_data_source_block           4MeOPyNO_1
_cod_depositor_comments
'Adding full bibliography for 7224402--7224408.cif.'
_cod_original_cell_volume        3787.28(13)
_cod_database_code               7224405
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H20 N4 O9'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2(H2), C2A(H2A), C4A(H4A), C5(H5), C5A(H5A), C9(H9), C12(H12)
2.c Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O6(H6), O11(H11), O13(H13)
;
_shelx_res_checksum              25425
_olex2_submission_special_instructions 'No special instructions were received'