Synthesis of Zigzag-Chain and Cyclic-Octanuclear Calcium Complexes and Hexanuclear Bulky Aryl-Phosphate Sodium Complexes with Ortho-Amide Groups: Structural Transformation Involving a Network of Inter- and Intramolecular Hydrogen Bonds
Akira Onoda; Yusuke Yamada; Taka-aki Okamura; Mototsugu Doi; Hitoshi Yamamoto; Norikazu Ueyama; Journal of the American Chemical Society 124 (2002) 1052–1059; doi:10.1021/ja011457r

data_4114602
_publ_section_title
;
 Synthesis of Zigzag-Chain and Cyclic-Octanuclear Calcium Complexes and
 Hexanuclear Bulky Aryl-Phosphate Sodium Complexes with Ortho-Amide
 Groups: Structural Transformation Involving a Network of Inter- and
 Intramolecular Hydrogen Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1052
_journal_page_last               1059
_journal_paper_doi               10.1021/ja011457r
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C28 H36 N3 O6 P'
_chemical_formula_weight         541.57
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.678(6)
_cell_length_b                   31.752(11)
_cell_length_c                   9.380(6)
_cell_measurement_temperature    296
_cell_volume                     5563(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.800
_diffrn_measured_fraction_theta_max 0.800
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.3040
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5806
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.145
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_F_000             2304
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.3211
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.2483
_reflns_number_gt                1332
_reflns_number_total             5132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011457r_3.cif
_cod_data_source_block           shelxl
_cod_database_code               4114602