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_7214081
_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 Er N12 O8, C12 H24 O6, 3(H2 O), H4 N 
;
_chemical_formula_sum            'C28 H50 Er N13 O17'
_chemical_formula_weight         1008.07
_chemical_name_common            NH4[Er(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                 112.9000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2104(6)
_cell_length_b                   24.2021(12)
_cell_length_c                   14.0890(7)
_cell_measurement_reflns_used    7469
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.21
_cell_volume                     4149.5(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 0.996
_diffrn_measured_fraction_theta_max 0.993
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29232
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    2.107
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         12052
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0653
_reflns_number_gt                9995
_reflns_number_total             12052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42031k.txt
_cod_data_source_block           NH4Er
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7214081