Supramolecular networks formation in crystals of 3-carboxybenzylphosphonic acid, its complexes and salts: from coordination bonds to weak intermolecular interactions
Dobrzyńska, Danuta; Kubiak, Joanna; Janczak, Jan; Zoń, Jerzy; RSC Advances 3 (2013) 23119–; doi:10.1039/c3ra44614j

data_7239303
_publ_section_title
;
 Supramolecular networks formation in crystals of
 3-carboxybenzylphosphonic acid, its complexes and salts: from
 coordination bonds to weak intermolecular interactions
;
_journal_issue                   45
_journal_name_full               'RSC Advances'
_journal_page_first              23119
_journal_paper_doi               10.1039/c3ra44614j
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C16 H24 Ca O14 P2, C10 H8 N2'
_chemical_formula_sum            'C26 H32 Ca N2 O14 P2'
_chemical_formula_weight         698.56
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                85.39(1)
_cell_angle_beta                 84.54(1)
_cell_angle_gamma                85.06(2)
_cell_formula_units_Z            1
_cell_length_a                   4.9848(10)
_cell_length_b                   6.5942(13)
_cell_length_c                   22.857(5)
_cell_measurement_reflns_used    525
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.69
_cell_volume                     743.2(3)
_computing_cell_refinement
;
Oxford Diffraction Poland, CrysAlis Red, Version 171.32.6, 2008
;
_computing_data_collection
;
Oxford Diffraction Poland, CrysAlis CCD, Version 171.32.6, 2008
;
_computing_data_reduction
;
Oxford Diffraction Poland, CrysAlis Red, Version 171.32.6, 2008
;
_computing_molecular_graphics
;
Brandenburg & Putz, DIAMOND Version 3.0, Crystal Impact GbR,
Bonn, Germany, (2006)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       \w-scan
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.1854
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9903
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.9061
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Oxford Diffraction Poland, CrysAlis Red, Version 171.32.6, 2008
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_meas      1.56
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.062(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3646
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1539
_refine_ls_R_factor_gt           0.0795
_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^)+(0.0800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1689
_reflns_number_gt                1929
_reflns_number_total             3646
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3ra44614j.txt
_cod_data_source_block           COMP4
_cod_database_code               7239303