Newin SituCondensation Reaction of Amino Diphosphonic Acids: A Series of Bicyclic Phosphonate Derivatives and Three Novel Water Clusters
Chen, Shuo-ping; Huang, Guang-xi; Li, Ming; Pan, Ling-ling; Yuan, Yi-xuan; Yuan, Liang-jie; Crystal Growth & Design 8 (2008) 2824–; doi:10.1021/cg7011149

data_4503425
_publ_section_title
;
 Newin SituCondensation Reaction of Amino Diphosphonic Acids: A Series of
 Bicyclic Phosphonate Derivatives and Three Novel Water Clusters
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2824
_journal_paper_doi               10.1021/cg7011149
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C72 H152 N42 Ni3 O44 P8'
_chemical_formula_weight         2734.25
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                64.0650(10)
_cell_angle_beta                 79.1050(10)
_cell_angle_gamma                73.9580(10)
_cell_formula_units_Z            1
_cell_length_a                   12.8261(8)
_cell_length_b                   16.6458(11)
_cell_length_c                   17.1892(11)
_cell_measurement_reflns_used    8234
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      2.28
_cell_volume                     3161.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21148
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.8029
_exptl_absorpt_correction_T_min  0.7711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1434
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         14686
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1107P)^2^+1.0532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1799
_reflns_number_gt                11459
_reflns_number_total             14686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg7011149-file005.cif
_cod_data_source_block           70315csp_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4503425