A redetermination of the crystal structure of the mannitol complex NH~4~[Mo~2~O~5~(C~6~H~11~O~6~)]·H~2~O: hydrogen-bonding scheme and Hirshfeld surface analysis
Mirzaei, Masoud; Tahmasebi, Morteza; Mague, Joel T.; Acta Crystallographica Section E 76 (2020) 518–522; doi:10.1107/S2056989020002935

data_2243314
_publ_section_title
;
 A redetermination of the crystal structure of the mannitol complex
 NH~4~[Mo~2~O~5~(C~6~H~11~O~6~)]&#x00B7;H~2~O: hydrogen-bonding scheme and
 Hirshfeld surface analysis
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              518
_journal_page_last               522
_journal_paper_doi               10.1107/S2056989020002935
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac          'N H4 [Mo2 (C6 H11 O6) O5], H2 O'
_chemical_formula_moiety         'H4 N +, C6 H11 Mo2 O11 -, H2 O'
_chemical_formula_sum            'C6 H17 Mo2 N O12'
_chemical_formula_weight         487.08
_chemical_name_systematic
'Ammonium \m-oxido-\m-[1,5,6-trihydroxyhexane-2,3,4-tris(olato)]bis[dioxidomolybdenum(V)] monohydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 99.664(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1775(17)
_cell_length_b                   6.7722(14)
_cell_length_c                   12.305(3)
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.624
_cell_measurement_theta_min      2.526
_cell_volume                     671.8(3)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12645
_diffrn_reflns_theta_full        29.500
_diffrn_reflns_theta_max         29.624
_diffrn_reflns_theta_min         1.679
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.513
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1454 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013).
;
_refine_ls_abs_structure_Flack   -0.026(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3598
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0187
_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^)+(0.0303P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                3407
_reflns_number_total             3598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7879sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        671.8(2)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2243314
_cod_database_fobs_code          2243314
_shelx_estimated_absorpt_t_min   0.611
_shelx_estimated_absorpt_t_max   0.881
_shelx_hkl_checksum              40967
_shelx_res_checksum              53465