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_2103427
_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                   6.6404(6)
_cell_length_b                   6.8981(5)
_cell_length_c                   15.9872(9)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      44.2
_cell_measurement_theta_min      32.7
_cell_volume                     732.31(9)
_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      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius MACH3'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         rotating-anode
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3283
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         69.88
_diffrn_reflns_theta_min         5.53
_diffrn_standards_decay_%        15.
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    12.88
_exptl_absorpt_correction_T_max  0.48
_exptl_absorpt_correction_T_min  0.22
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
ABSPSI, (Alcock and Marks, 1994)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.370
_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          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.579
_refine_ls_extinction_coef       0.00379(19)
_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   1.339
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.339
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+0.2678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0456
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.046
_reflns_number_gt                751
_reflns_number_total             757
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br0112.cif
_cod_data_source_block           2
_cod_database_code               2103427
_cod_database_fobs_code          2103427