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_7224407
_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(C11 H9 N O), C32 H32 O8'
_chemical_formula_sum            'C54 H50 N2 O10'
_chemical_formula_weight         886.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-25
_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                 100.307(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3203(4)
_cell_length_b                   16.1527(4)
_cell_length_c                   20.8931(4)
_cell_measurement_reflns_used    5047
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      74.2060
_cell_measurement_theta_min      4.3200
_cell_volume                     4422.79(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w   -115.00 -25.00   1.00   20.00    --  -41.78 -37.00-180.00   90
  2  \w    -96.00  -7.00   1.00   20.00    --  -41.78 125.00 -30.00   89
  3  \w     18.00  46.00   1.00   20.00    --   41.78 -37.00-120.00   28
  4  \w     74.00 174.00   1.00   80.00    --  106.66  77.00-180.00  100
  5  \w    105.00 178.00   1.00   80.00    --  106.66 125.00  60.00   73
  6  \w     32.00 135.00   1.00   80.00    --  106.66 -77.00  90.00  103
  7  \w     42.00 119.00   1.00   80.00    --  106.66 -45.00 -90.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0180660000
_diffrn_orient_matrix_UB_12      -0.0658168000
_diffrn_orient_matrix_UB_13      0.0541739000
_diffrn_orient_matrix_UB_21      -0.0344795000
_diffrn_orient_matrix_UB_22      0.0619215000
_diffrn_orient_matrix_UB_23      0.0477330000
_diffrn_orient_matrix_UB_31      -0.1109995000
_diffrn_orient_matrix_UB_32      -0.0301548000
_diffrn_orient_matrix_UB_33      -0.0202376000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12192
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         66.748
_diffrn_reflns_theta_min         3.372
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         12192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0609P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7976
_reflns_number_total             12192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00240d2.cif
_cod_data_source_block           4PhPyNO_1
_cod_depositor_comments
'Adding full bibliography for 7224402--7224408.cif.'
_cod_original_cell_volume        4422.80(19)
_cod_database_code               7224407
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H20 N1 O9'
_reflns_odcompleteness_completeness 98.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7434(6) 0.2566(6)
2. 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
3.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28)
3.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C2(H2), C2A(H2A), C2B(H2B), C4A(H4A), C4B(H4B), C5(H5),
 C5A(H5A), C5B(H5B), C7A(H7A), C7B(H7B), C8A(H8A), C8B(H8B), C9(H9), C9A(H9A),
 C9B(H9B), C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B), C12(H12), C16(H16),
 C19(H19), C23(H23), C26(H26)
3.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C)
3.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O6(H6), O11(H11), O13(H13), O18(H18), O20(H20), O25(H25), O27(H27)
;
_shelx_res_checksum              34140
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.454
_oxdiff_exptl_absorpt_empirical_full_min 0.750