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_4114600
_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            'C53 H76 N5 Na3 O20 P2'
_chemical_formula_weight         1234.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                114.6090(10)
_cell_angle_beta                 109.742(5)
_cell_angle_gamma                71.321(2)
_cell_formula_units_Z            2
_cell_length_a                   15.1649(13)
_cell_length_b                   16.8922(16)
_cell_length_c                   14.3956(10)
_cell_measurement_temperature    173
_cell_volume                     3085.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21113
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.167
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             1304
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         13267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0715
_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          0.1956
_refine_ls_wR_factor_ref         0.2111
_reflns_number_gt                8448
_reflns_number_total             13273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011457r_1.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3085.4(4)
_cod_database_code               4114600