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_7214083
_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 H28 K O8, H2 O 
;
_chemical_formula_sum            'C28 H46 Dy K N12 O17'
_chemical_formula_weight         1024.37
_chemical_name_common            '[Dy(cdm)4(H2O)4][K(18c6)(H2O)2].H2O'
_chemical_name_systematic
; 
 ? 
;
_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                 112.8950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2831(6)
_cell_length_b                   24.0971(12)
_cell_length_c                   13.9960(6)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.08
_cell_measurement_theta_min      2.37
_cell_volume                     4127.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            36531
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    1.995
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.490
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         11127
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+4.8917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                10089
_reflns_number_total             11127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42031k.txt
_cod_data_source_block           KDy
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7214083