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_7035067
_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
'C10 H10 Cl2 Cu N2 O2, 2(C40 H48 O8), 2(C H4 O), 2(C H3 O)'
_chemical_formula_sum            'C94 H120 Cl2 Cu N2 O22'
_chemical_formula_weight         1764.35
_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
_audit_creation_date             2015-03-16
_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                105.26(3)
_cell_angle_beta                 101.94(3)
_cell_angle_gamma                97.56(3)
_cell_formula_units_Z            1
_cell_length_a                   12.163(2)
_cell_length_b                   12.630(3)
_cell_length_c                   16.953(3)
_cell_measurement_temperature    170.0
_cell_volume                     2409.9(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_unetI/netI     0.1546
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30183
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.502
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0832 before and 0.0714 after correction.
The Ratio of minimum to maximum transmission is 0.8369.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       needle
_exptl_crystal_F_000             937
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         8720
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      2.442
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0765
_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^)+(0.1028P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5243
_reflns_number_total             8720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01143d2.cif
_cod_data_source_block           IV
_cod_depositor_comments
'Adding full bibliography for 7035064--7035069.cif.'
_cod_original_cell_volume        2410.0(9)
_cod_database_code               7035067
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H3 of O3, H5 of O5, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8, H4 of O4, H15 of O15, All C(H,H,H,H,H,H)
  groups, All Cl(H) groups
2. Restrained distances
 O15-H15
 0.85 with sigma of 0.02
 O5-O6
 0.85 with sigma of 0.02
 H5-O5
 0.85 with sigma of 0.02
 O3-H3
 0.85 with sigma of 0.02
 O10-C47
 1.47 with sigma of 0.02
 H7-O7
 0.85 with sigma of 0.02
 O6-H6
 0.85 with sigma of 0.02
 H8-O8
 0.85 with sigma of 0.02
 H2-O2
 0.85 with sigma of 0.02
 H5-O5
 0.85 with sigma of 0.02
 O11-C47
 1.45 with sigma of 0.02
 O10-C47
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O11) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: O10(0.85) O11(0.15) H47A(0.85) H47B(0.85) H47C(0.85) H47D(0.15)
 H47E(0.15) H47F(0.15)
5.a Me refined with riding coordinates:
 C47(H47A,H47B,H47C), C47(H47D,H47E,H47F)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              10693
_olex2_submission_special_instructions 'No special instructions were received'