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_7214085
_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         1003.28
_chemical_name_common            NH4[Dy(cdm)4(H2O)4].18c6.3H2O
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 112.907(4)
_cell_angle_gamma                90
_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_temperature    123(2)
_cell_volume                     4161.2(3)
_computing_cell_refinement       'LaueG (Piltz, 2011)'
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
;
argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'From X-ray data'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.765
_diffrn_measured_fraction_theta_max 0.755
_diffrn_measurement_details      '30 images, exposure time 40 minutes'
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.85-1.7
_diffrn_reflns_av_R_equivalents  0.1122
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.765
_diffrn_reflns_Laue_measured_fraction_max 0.755
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            112955
_diffrn_reflns_point_group_measured_fraction_full 0.765
_diffrn_reflns_point_group_measured_fraction_max 0.755
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.453
_diffrn_reflns_theta_min         1.871
_diffrn_source                   'nuclear reactor'
_diffrn_source_details           'thermal neutrons, supermirror guides'
_diffrn_source_type              'OPAL reactor, ANSTO, Lucas Heights, Australia'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       block
_exptl_crystal_F_000             945
_exptl_crystal_size_max          1.2
_exptl_crystal_size_mid          1.0
_exptl_crystal_size_min          1.0
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.675
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         7928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.675
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0750
_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^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6418
_reflns_number_total             7928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce42031k.txt
_cod_data_source_block           NH4DyNeut
_cod_database_code               7214085
_diffrn_detector_area_resol_max  1.33
_shelxl_version_number           2013-2
_shelx_res_checksum              23950
_shelx_hkl_checksum              18475