<i>In situ</i> decarbonylation of <i>N</i>,<i>N</i>-dimethylformamide to form dimethylammonium cations in the hybrid framework compound {[(CH~3~)~2~NH~2~]~2~[Zn{O~3~PC~6~H~2~(OH)~2~PO~3~}]}~<i>n~</i>
Soriano, Josemaria S.; Galeas, Bryan E.; Garrett, Paul; Flores, Ryan A.; Pinedo, Juan L.; Kohlgruber, Tsuyoshi A.; Felton, Daniel; Adelani, Pius O.; Acta Crystallographica Section E 75 (2019) 1540–1543; doi:10.1107/S2056989019012969

data_2243606
_publ_section_title
;
 <i>In situ</i> decarbonylation of <i>N</i>,<i>N</i>-dimethylformamide to
 form dimethylammonium cations in the hybrid framework compound
 {[(CH~3~)~2~NH~2~]~2~[Zn{O~3~PC~6~H~2~(OH)~2~PO~3~}]}~<i>n~</i>
;
_journal_coeditor_code           HB7847
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1540
_journal_page_last               1543
_journal_paper_doi               10.1107/S2056989019012969
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '(C2 H8 N)2 [Zn (C6 H4 O8 P2)]'
_chemical_formula_moiety         'C10 H20 N2 O8 P2 Zn'
_chemical_formula_sum            'C10 H20 N2 O8 P2 Zn'
_chemical_formula_weight         423.59
_chemical_name_systematic
;
Poly[bis(dimethylammonium)
[(\m~4~-2,5-dihydroxybenzene-1,4-diphosphonato)zinc(II)]]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 97.3380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8455(5)
_cell_length_b                   16.4492(9)
_cell_length_c                   11.2721(6)
_cell_measurement_reflns_used    8723
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.20
_cell_volume                     1626.67(15)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008a)
;
_computing_publication_material
;
<i>CIFTAB</i> (Sheldrick, 2008b)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19692
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.969
_diffrn_reflns_theta_min         2.203
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.308
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.4955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                3582
_reflns_number_total             4040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7847sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243606
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.949
_shelx_hkl_checksum              64113
_shelx_res_checksum              29194
_cod_database_fobs_code 2243606