Coordination Polymers Utilizing N-Oxide Functionalized Host Ligands
James J. Henkelis; Sarah A. Barnett; Lindsay P. Harding; Michaele J. Hardie; Inorganic Chemistry 51 (2012) 10657–10674; doi:10.1021/ic300940k

data_4330598
_publ_section_title
;
 Coordination Polymers Utilizing N-Oxide Functionalized Host Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10657
_journal_page_last               10674
_journal_paper_doi               10.1021/ic300940k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C42 H43 N3 O11'
_chemical_formula_weight         765.79
_chemical_name_systematic
; 
(\+-)-2,7,12-Trimethoxy-3,8,13-tris(2-N-oxide-pyridylmethoxy)-
10,15-dihydro-5H- tribenzo[a,d,g]cyclononatriene
hydrate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.660(4)
_cell_angle_beta                 92.270(4)
_cell_angle_gamma                92.770(4)
_cell_formula_units_Z            2
_cell_length_a                   4.5584(6)
_cell_length_b                   16.3294(18)
_cell_length_c                   24.986(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1829.2(4)
_computing_cell_refinement       'CELL_NOW (Bruker)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'TWINABS (Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'BRUKER X8 CCD area detector'
_diffrn_measurement_method       '\w, \p-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_sigmaI/netI    0.1528
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22009
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.9919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       fragment
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2.7(16)
_refine_ls_extinction_coef       0.015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         11097
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1373P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2175
_refine_ls_wR_factor_ref         0.2440
_reflns_number_gt                6454
_reflns_number_total             11097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300940k_si_002_04.cif
_cod_data_source_block           c:'L3_2H2O'
_cod_database_code               4330598