A ladder coordination polymer based on Ca^2+^ and (4,5-dicyano-1,2-phenylene)bis(phosphonic acid): crystal structure and solution-state NMR study
Venkatramaiah, Nutalapati; Mendes, Ricardo F.; Silva, Artur M. S.; Tomé, João P. C.; Almeida Paz, Filipe A.; Acta Crystallographica Section C 72 (2016) –; doi:10.1107/S2053229616012328

data_2020583
_publ_section_title
;
 A ladder coordination polymer based on Ca^2+^ and
 (4,5-dicyano-1,2-phenylene)bis(phosphonic acid): crystal structure and
 solution-state NMR study
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229616012328
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Ca2 (C8 H4 N2 O6 P2 )2 (H2 O)2], 4H2 O'
_chemical_formula_moiety         'C16 H12 Ca2 N4 O14 P4, 4(H2 O)'
_chemical_formula_sum            'C16 H20 Ca2 N4 O18 P4'
_chemical_formula_weight         760.40
_chemical_name_systematic
'Poly[[diaqua[\m~4~-(4,5-dicyano-1,2-phenylene)bis(phosphonato)][\m~3~-(4,5-dicyano-1,2-phenylene)bis(phosphonato)]dicalcium(II)] tetrahydrate]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'SHELXL-2014/6, manual editing plus enCIFer'
_cell_angle_alpha                90
_cell_angle_beta                 91.493(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4384(11)
_cell_length_b                   25.2929(18)
_cell_length_c                   6.9599(5)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.48
_cell_volume                     2892.8(4)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w / \f scans'
_diffrn_radiation_monochromator  'Multi-layer X-ray mirror'
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            27705
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         3.591
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.462
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         5266
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+10.5068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                4050
_reflns_number_total             5266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yf3107sup1.cif
_cod_data_source_block           I
_cod_database_code               2020583
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.993
_shelx_hkl_checksum              45469
_shelx_res_checksum              41684
_shelxl_version_number           2014/6
_cod_database_fobs_code 2020583