A detailed comparative structural study of the hydrogen bonded networks in solids, obtained by the reaction of 4,4′-bipyridine and varied alkane-α,ω-diphosphonic acids
van Megen, M.; Frank, W.; Reiss, G. J.; CrystEngComm 18 (2016) 3574–; doi:10.1039/C5CE02156A

data_7225065
_publ_section_title
;
 A detailed comparative structural study of the hydrogen bonded networks
 in solids, obtained by the reaction of 4,4&#x2032;-bipyridine and varied
 alkane-\a,\w-diphosphonic acids
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              3574
_journal_paper_doi               10.1039/C5CE02156A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C28 H52 N2 O12 P4'
_chemical_formula_weight         732.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-10-25 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.59(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   42.860(9)
_cell_length_b                   11.426(2)
_cell_length_c                   7.3826(15)
_cell_measurement_reflns_used    12351
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.913
_cell_measurement_theta_min      2.020
_cell_volume                     3615.2(12)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  Xcalibur-EOS
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            26931
_diffrn_reflns_point_group_measured_fraction_full 0.831
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.913
_diffrn_reflns_theta_min         2.020
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.267
_exptl_absorpt_correction_T_min  0.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   shelxl
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 3796 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         12351
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+3.3292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.661
_reflns_Friedel_fraction_full    0.683
_reflns_Friedel_fraction_max     0.627
_reflns_number_gt                11004
_reflns_number_total             12351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02156a2.cif
_cod_data_source_block           no_311
_cod_depositor_comments
'Adding full bibliography for 7225062--7225069.cif.'
_cod_database_code               7225065
_shelxl_version_number           2014-3
_shelx_res_checksum              67601