Aminoguanidinium(1+) pentafluorozirconate: multiple redetermination and comparisons
Ross II, C. R.; Bauer, M. R.; Nielson, R. M.; Abrahams, S. C.; Acta Crystallographica Section B 58 (2002) 841–848; doi:10.1107/S0108768102012624

data_2103428
_publ_section_title
;
 Aminoguanidinium(1+) pentafluorozirconate: multiple redetermination
 and comparisons
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              841
_journal_page_last               848
_journal_paper_doi               10.1107/S0108768102012624
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C H7 N4 1+, F5 Zr 1-'
_chemical_formula_structural     '(C N4 H7) Zr F5'
_chemical_formula_sum            'C H7 F5 N4 Zr'
_chemical_formula_weight         261.33
_chemical_name_common            'aminoguanidinium pentafluorozirconate'
_chemical_name_systematic        'aminoguanidinium pentafluorozirconate'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6485(4)
_cell_length_b                   6.9340(4)
_cell_length_c                   16.0344(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    283(2)
_cell_measurement_theta_max      23.888
_cell_measurement_theta_min      20.056
_cell_volume                     739.20(6)
_computing_cell_refinement       'CAD4 Express (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD4 Express (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_molecular_graphics    'ORTEP-III (Burnett and Johnson, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      283.0(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius MACH3'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71065
_diffrn_reflns_av_R_equivalents  0.0099
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3001
_diffrn_reflns_theta_full        29.94
_diffrn_reflns_theta_max         29.95
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_density_meas      2.305(5)
_exptl_crystal_density_method    pycnometric
_exptl_crystal_description       blocky
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.290
_refine_ls_extinction_coef       0.0073(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0167
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0087P)^2^+0.1490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0408
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0408
_reflns_number_gt                1076
_reflns_number_total             1159
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br0112.cif
_cod_data_source_block           3
_cod_database_code               2103428
_cod_database_fobs_code          2103428