A neutron diffraction study of hydrogen bonding in isostructural potassium and ammonium lanthanoidates
Emerson, Adrian J.; Edwards, Alison J.; Batten, Stuart R.; Turner, David R.; CrystEngComm 16 (2014) 1625–; doi:10.1039/c3ce42031k

data_7214080
_publ_section_title
;
 A neutron diffraction study of hydrogen bonding in isostructural
 potassium and ammonium lanthanoidates
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1625
_journal_paper_doi               10.1039/c3ce42031k
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
;
C16 H16 Dy N12 O8, C12 H24 O6, 3(H2 O), H4 N 
;
_chemical_formula_sum            'C28 H50 Dy N13 O17'
_chemical_formula_weight         1003.31
_chemical_name_common            NH4[Dy(cdm)4(H2O)4].18c6.3H2O
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.907(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2276(5)
_cell_length_b                   24.2200(8)
_cell_length_c                   14.1006(5)
_cell_measurement_reflns_used    8873
_cell_measurement_temperature    123.1(4)
_cell_measurement_theta_max      30.9226
_cell_measurement_theta_min      2.2947
_cell_volume                     4161.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123.1(4)
_diffrn_detector_area_resol_mean 10.3389
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25233
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.99
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.880
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.830
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         11602
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0194P)^2^+0.0073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                9512
_reflns_number_total             11602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42031k.txt
_cod_data_source_block           NH4Dy
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7214080