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_7035069
_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         '2(C40 H48 O8), C12 H8 Cu N2 O6, 4(H2 O), 2(O)'
_chemical_formula_sum            'C92 H112 Cu N2 O28'
_chemical_formula_weight         1757.37
_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     iterative
_audit_creation_date             2015-03-03
_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                81.845(4)
_cell_angle_beta                 73.601(5)
_cell_angle_gamma                69.069(5)
_cell_formula_units_Z            1
_cell_length_a                   12.1909(7)
_cell_length_b                   12.7422(6)
_cell_length_c                   15.5226(9)
_cell_measurement_reflns_used    3760
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.7680
_cell_measurement_theta_min      3.4160
_cell_volume                     2158.3(2)
_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, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -90.00   13.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2930  -19.0000   30.0000 103

  2 omega  -86.00   12.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2930  -77.0000 -150.0000 98

  3 omega  -28.00    1.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2930  -57.0000  -30.0000 29

  4 omega  -47.00   50.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2930   77.0000  -30.0000 97

  5 omega   15.00   61.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5430  -99.0000  120.0000 46

  6 omega   41.00   66.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5430 -107.0000  121.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0331426000
_diffrn_orient_matrix_UB_12      0.0066792000
_diffrn_orient_matrix_UB_13      0.0456293000
_diffrn_orient_matrix_UB_21      -0.0397659000
_diffrn_orient_matrix_UB_22      -0.0249892000
_diffrn_orient_matrix_UB_23      -0.0075509000
_diffrn_orient_matrix_UB_31      0.0382176000
_diffrn_orient_matrix_UB_32      -0.0537618000
_diffrn_orient_matrix_UB_33      0.0115997000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14471
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         3.048
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73156
_exptl_absorpt_correction_type   multi-scan
_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_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_F_000             931
_exptl_crystal_size_max          0.1543
_exptl_crystal_size_mid          0.1409
_exptl_crystal_size_min          0.0854
_refine_diff_density_max         0.839
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0755
_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^)+(0.1057P)^2^+3.7171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5613
_reflns_number_total             7807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01143d2.cif
_cod_data_source_block           VI
_cod_depositor_comments
'Adding full bibliography for 7035064--7035069.cif.'
_cod_database_code               7035069
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H20 N1 O9'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H3-O3
 0.85 with sigma of 0.02
 H2-O2
 0.85 with sigma of 0.02
 O4-H4
 0.85 with sigma of 0.02
 O5-H5
 0.85 with sigma of 0.02
 H1-O1
 0.85 with sigma of 0.02
 H8-O8
 0.85 with sigma of 0.02
 O6-H6
 0.85 with sigma of 0.02
 O15-H15A
 0.85 with sigma of 0.02
 H15B-O15
 0.85 with sigma of 0.02
 H14A-H14B
 0.85 with sigma of 0.02
 H14B-H14A
 0.85 with sigma of 0.02
 H14A-O14
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: O12(0.5) O13(0.5)
4.a Riding coordinates:
 O14(H14A,H14B)
4.b Ternary CH refined with riding coordinates:
 C8(H8A), C18(H18), C28(H28), C38(H38)
4.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C19(H19A,H19B), C29(H29A,H29B), C39(H39A,H39B)
4.d Aromatic/amide H refined with riding coordinates:
 C6(H6A), C16(H16), C26(H26), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44)
4.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C40(H40A,
 H40B,H40C)
;
_shelx_res_checksum              14328
_olex2_submission_special_instructions 'No special instructions were received'