Methylresorcinarene: a reaction vessel to control the coordination geometry of copper(ii) in pyridine N-oxide copper(ii) complexes.
Beyeh, Ngong Kodiah; Puttreddy, Rakesh; Dalton transactions (Cambridge, England : 2003) 44 (2015) 9881–9886; doi:10.1039/c5dt01143d

data_7035065
_publ_section_title
;
 Methylresorcinarene: a reaction vessel to control the coordination
 geometry of copper(ii) in pyridine N-oxide copper(ii) complexes.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9881
_journal_page_last               9886
_journal_paper_doi               10.1039/c5dt01143d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C40 H48 O8, C6 H5 N O3, 3(O)'
_chemical_formula_sum            'C46 H53 N O14'
_chemical_formula_weight         843.89
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-03-16 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                77.408(4)
_cell_angle_beta                 87.270(4)
_cell_angle_gamma                74.490(5)
_cell_formula_units_Z            2
_cell_length_a                   11.4574(6)
_cell_length_b                   11.5478(6)
_cell_length_c                   17.0220(8)
_cell_measurement_reflns_used    5449
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.2020
_cell_measurement_theta_min      3.9850
_cell_volume                     2117.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega    3.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000   30.0000 27

  2 omega  -43.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000   30.0000 32

  3 omega  -49.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000 -120.0000 81

  4 omega  -96.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  125.0000  -90.0000 94

  5 omega -115.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -57.0000   90.0000 100

  6 omega   80.00  171.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   30.0000  -60.0000 91

  7 omega  111.00  178.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   61.0000  -30.0000 67

  8 omega   53.00  144.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   15.0000   90.0000 91

  9 omega   40.00  109.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -94.0000  -60.0000 69

 10 omega   36.00   98.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -45.0000  -90.0000 62

 11 omega   35.00   87.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -45.0000 -180.0000 52

 12 omega   25.00  109.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -94.0000 -180.0000 84

 13 omega   31.00   91.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -30.0000   30.0000 60

 14 omega   30.00  131.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -77.0000   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      -0.0822138000
_diffrn_orient_matrix_UB_12      -0.0756418000
_diffrn_orient_matrix_UB_13      -0.0203508000
_diffrn_orient_matrix_UB_21      0.0464136000
_diffrn_orient_matrix_UB_22      0.0164825000
_diffrn_orient_matrix_UB_23      -0.0871040000
_diffrn_orient_matrix_UB_31      0.1027664000
_diffrn_orient_matrix_UB_32      -0.1186939000
_diffrn_orient_matrix_UB_33      0.0244866000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_laue_measured_fraction_full 0.971
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13282
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.733
_diffrn_reflns_theta_min         4.004
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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    1.323
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.1527
_exptl_crystal_size_min          0.1224
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         7430
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0853P)^2^+0.7245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5956
_reflns_number_total             7430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01143d2.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 7035064--7035069.cif.'
_cod_database_code               7035065
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C26 H17 O8 N2'
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.02
3. Others
 Sof(O14)=1-FVAR(1)
 Sof(O15)=FVAR(1)
 Fixed Sof: O12(0.5) O13(0.5) O19(0.45) O18(0.3) O16(0.15) O17(0.1)
4.a Riding coordinates:
 O1(H1)
4.b Ternary CH refined with riding coordinates:
 C18(H18), C8(H8A), C38(H38), C28(H28)
4.c Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C9(H9A,H9B), C29(H29A,H29B), C19(H19A,H19B)
4.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C5(H5A), C36(H36), C26(H26), C44(H44), C42(H42), C41(H41), C43(H43)
4.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C40(H40A,H40B,H40C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C37(H37A,
 H37B,H37C)
;
_shelx_res_checksum              17247
_olex2_submission_special_instructions 'No special instructions were received'