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_4114604
_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_moiety         'C208 H278 Ca8 N32 O87 P8 '
_chemical_formula_sum            'C208 H278 Ca8 N32 O87 P8'
_chemical_formula_weight         5187.02
_chemical_name_systematic
; 
[Ca8(O3POC6H3(NHCOPh)2)8(H2O)12(dmf)8]-8(DMF)-11(H2O)
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      85
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Fri Aug 31 10:24:09 2001'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   29.8134(5)
_cell_length_b                   29.8134(5)
_cell_length_c                   16.9925(3)
_cell_measurement_reflns_used    89508
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     15103.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR88 (Burla, 1989)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_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    0.1454
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17887
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    0.260
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             5452
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         17290
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.805
_refine_ls_R_factor_all          0.2491
_refine_ls_R_factor_gt           0.1052
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2860
_refine_ls_wR_factor_ref         0.3395
_reflns_number_gt                3918
_reflns_number_total             17290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011457r_5.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4114604