Supramolecular Isomerism and Isomorphism in the Structures of 1,4-Butanebisphosphonic Acid and Its Organic Ammonium Salts
Mahmoudkhani, Amir H.; Langer, Vratislav; Crystal Growth & Design 2 (2002) 21–; doi:10.1021/cg015553f

data_4505774
_publ_section_title
;
 Supramolecular Isomerism and Isomorphism in the Structures of
 1,4-Butanebisphosphonic Acid and Its Organic Ammonium Salts
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              21
_journal_paper_doi               10.1021/cg015553f
_journal_volume                  2
_journal_year                    2002
_chemical_formula_sum            'C28 H34 N6 O6 P2'
_chemical_formula_weight         612.55
_chemical_name_systematic
; 
p-Phenylazoanilinium butanebisphosphonate 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.291(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   65.3761(8)
_cell_length_b                   6.3533(1)
_cell_length_c                   7.4586(1)
_cell_measurement_reflns_used    5699
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      1
_cell_volume                     3097.92(7)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT & SADABS'
_computing_molecular_graphics    'Diamond (Brandenburg, 2000)'
_computing_structure_refinement  'SHELXTL (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXTL (Bruker AXS, 2001)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       '\w 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  0.028
_diffrn_reflns_av_sigmaI/netI    0.027
_diffrn_reflns_limit_h_max       73
_diffrn_reflns_limit_h_min       -72
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9494
_diffrn_reflns_theta_full        24.02
_diffrn_reflns_theta_max         24.02
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.9962
_exptl_absorpt_correction_T_min  0.9192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2277
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.047
_refine_ls_R_factor_gt           0.037
_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^)+(0.0510P)^2^+2.6150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.095
_refine_ls_wR_factor_ref         0.102
_reflns_number_gt                1939
_reflns_number_total             2277
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cg015553f_s1.cif
_cod_data_source_block           n
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4505774