Heavier alkali metal complexes of 2-phenylamidopyridine: An X-ray crystallographic and theoretical study of a structurally diverse series of crown ether adducts
Liddle, Stephen T.; Clegg, William; Morrison, Carole A.; Dalton Transactions  (2004) 2514–2525; doi:10.1039/b406741j

data_7027872
_publ_section_title
;
 Heavier alkali metal complexes of 2-phenylamidopyridine: An X-ray
 crystallographic and theoretical study of a structurally diverse series
 of crown ether adducts
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              2514
_journal_page_last               2525
_journal_paper_doi               10.1039/b406741j
_journal_year                    2004
_chemical_formula_moiety         'C20 H40 O9 Rb +,C11 H9 N2 -'
_chemical_formula_sum            'C31 H49 N2 O9 Rb'
_chemical_formula_weight         679.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.718(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   36.589(4)
_cell_length_b                   11.3191(12)
_cell_length_c                   26.225(3)
_cell_measurement_reflns_used    6051
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.46
_cell_volume                     10158.8(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8835
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.514
_exptl_absorpt_correction_T_max  0.461
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4296
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.78
_exptl_crystal_size_min          0.62
_refine_diff_density_max         1.518
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         8835
_refine_ls_number_restraints     3227
_refine_ls_restrained_S_all      1.743
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1181P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1751
_reflns_number_gt                6283
_reflns_number_total             8835
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b406741jsup1.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7027872