5-Aminonaphthalene-1-sulfonic acid and its manganese, nickel and cobalt salts
Genther, Dane J.; Squattrito, Philip J.; Kirschbaum, Kristin; Yearley, Eric J.; Pinkerton, A. Alan; Acta Crystallographica Section C 63 (2007) m604–m609; doi:10.1107/S0108270107052286

data_2016356
_publ_section_title
;
 5-Aminonaphthalene-1-sulfonic acid and its manganese, nickel and
 cobalt salts
;
_journal_coeditor_code           SK3173
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m604
_journal_page_last               m609
_journal_paper_doi               10.1107/S0108270107052286
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni (H2 O)6] (C10 H8 N O3 S)2 , 3H2 O'
_chemical_formula_moiety         'H12 Ni O6 2+ , 2C10 H8 N O3 S - , 3H2 O'
_chemical_formula_sum            'C20 H34 N2 Ni O15 S2'
_chemical_formula_weight         665.32
_chemical_name_common
;
hexaaquanickel(II) 5-aminonaphthalene-1-sulfonate trihydrate
;
_chemical_name_systematic
;
hexaaquanickel(II) bis(5-aminonaphthalene-1-sulfonate) trihydrate
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1031(6)
_cell_length_b                   22.9375(18)
_cell_length_c                   7.4607(6)
_cell_measurement_reflns_used    5158
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.73
_cell_volume                     1386.68(19)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000) and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 6000 CCD area-detector'
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14174
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS and SAINT-Plus; Bruker, 2003)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.265
_refine_ls_abs_structure_details 'Flack (1983), with 1433 Friedel pairs'
_refine_ls_abs_structure_Flack   0.072(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3435
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0269P)^2^+0.3548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                3309
_reflns_number_total             3435
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3173.cif
_cod_data_source_block           III
_cod_database_code               2016356
_cod_database_fobs_code          2016356