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_4114601
_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            'C26 H32 N3 O6 P'
_chemical_formula_weight         513.53
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_symmetry_cell_setting           triclinic
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_symmetry_space_group_name_Hall  '-P 1'
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_cell_angle_alpha                100.79(2)
_cell_angle_beta                 108.64(1)
_cell_angle_gamma                78.99(2)
_cell_formula_units_Z            2
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_cell_length_b                   14.612(3)
_cell_length_c                   8.142(1)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.0
_cell_volume                     1305.7(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    directMethod
_diffrn_measured_fraction_theta_full 1.0000
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_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_av_R_equivalents  0.015
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_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
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_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.150
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_exptl_crystal_description       prismatic
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_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         2170
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.0073
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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_cod_data_source_block           onoda6
_cod_original_cell_volume        1305.6(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C26 H32 N3 O6 P '
_cod_database_code               4114601