New Molecular Perovskites: Cubic C4N2H12.NH4Cl3.H2O and 2-H Hexagonal C6N2H14.NH4Cl3
Colin A. Bremner; Michael Simpson; William T. A. Harrison; Journal of the American Chemical Society 124 (2002) 10960–10961; doi:10.1021/ja027484e

data_4115144
_publ_section_title
;
 New Molecular Perovskites: Cubic C4N2H12.NH4Cl3.H2O and 2-H Hexagonal
 C6N2H14.NH4Cl3
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10960
_journal_page_last               10961
_journal_paper_doi               10.1021/ja027484e
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         '(C4, N2, H12)(N H4)Cl3(H2 O)'
_chemical_formula_sum            'C4 H18 Cl3 N3 O'
_chemical_formula_weight         230.56
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5279(13)
_cell_length_b                   12.935(3)
_cell_length_c                   12.849(3)
_cell_measurement_reflns_used    2660
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.48
_cell_measurement_theta_min      3.1
_cell_volume                     1084.9(4)
_computing_cell_refinement       'Bruker SMART software (Bruker, 1999a)'
_computing_data_collection       'Bruker SMART software (Bruker, 1999a)'
_computing_data_reduction        'Bruker SMART software (Bruker, 1999a)'
_computing_molecular_graphics    'ATOMS (Shape software, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       \w
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8891
_diffrn_reflns_theta_full        32.47
_diffrn_reflns_theta_max         32.47
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0106(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         2032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0454P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                1453
_reflns_number_total             2032
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja027484e_s1_1.cif
_cod_data_source_block           cubic
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap and geom' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1085.0(4)
_cod_original_formula_sum        'C4 H18 Cl3 N3 O1'
_cod_database_code               4115144