Probing ferroic transitions in a multiferroic framework family: a neutron diffraction study of the ammonium transition metal formates.
Lawler, James M. M.; Manuel, Pascal; Thompson, Amber L.; Saines, Paul J.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11613–11620; doi:10.1039/c5dt00733j

data_7035273
_publ_section_title
;
 Probing ferroic transitions in a multiferroic framework family: a neutron
 diffraction study of the ammonium transition metal formates.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11613
_journal_page_last               11620
_journal_paper_doi               10.1039/c5dt00733j
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_compound_source        synthesised
_chemical_formula_moiety         'C3 H3 Mn O6, H4 N'
_chemical_formula_sum            'C3 H7 Mn N O6'
_chemical_formula_weight         208.02
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2015-02-10 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8568(2)
_cell_length_b                   9.3906(2)
_cell_length_c                   10.7307(3)
_cell_measurement_reflns_used    950
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     690.94(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9149
_diffrn_reflns_theta_full        27.472
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         5.263
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.895
_exptl_absorpt_correction_T_max  2.15285
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.41
_refine_ls_extinction_coef       62(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9596
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1481
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.0001083
_refine_ls_shift/su_mean         0.0000155
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.99P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0641
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0641
_reflns_limit_h_max              8
_reflns_limit_h_min              0
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                1335
_reflns_number_total             1481
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.27
_oxford_diffrn_Wilson_scale      4.58
_oxford_refine_ls_r_factor_ref   0.0327
_oxford_refine_ls_scale          0.4367(10)
_oxford_reflns_number_all        1481
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c5dt00733j2.cif
_cod_data_source_block           Mn-Formate_new_polymorph
_cod_depositor_comments
'Adding full bibliography for 7035273--7035275.cif.'
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C3 H7 Mn1 N1 O6'
_cod_database_code               7035273
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
REM TOO MANY H ATOMS ON N   (  11), - 4 
RIDE N   (  11,X'S) H   ( 114,X'S) H   ( 113,X'S) H   ( 112,X'S) H   ( 111,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;