Crystal structure of tris(1,10-phenanthroline)nickel(II) bis(o-aminobenzenesulfonate) — ethanol (1:1), [Ni(C12H8N2)3][C6H6NO3S]2 · C2H5OH, at 120 K
Bernard Tinant; François Robert; Yann Garcia; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 546–; doi:

data_8102790
_publ_section_title
;
 Crystal structure of tris(1,10-phenanthroline)nickel(II)
 bis(o-aminobenzenesulfonate) --- ethanol (1:1),
 [Ni(C12H8N2)3][C6H6NO3S]2 &#x00B7; C2H5OH, at 120 K
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              546
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety
'C36 H24 N6 Ni, 0.5(C12 H12 N2 O6 S2), C6 H6 N O3 S, C2 H6 O'
_chemical_formula_sum            'C50 H42 N8 Ni O7 S2'
_chemical_formula_weight         989.75
_chemical_name_systematic
; 
tris(1,10-phenanthroline)-nickel(ii) bis 
o-aminobenzenesulfonate ethanol solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.70
_cell_angle_beta                 74.52
_cell_angle_gamma                71.69
_cell_formula_units_Z            2
_cell_length_a                   11.709(2)
_cell_length_b                   13.200(5)
_cell_length_c                   15.544(3)
_cell_measurement_reflns_used    32314
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      3.
_cell_volume                     2127.4(10)
_computing_cell_refinement       MAR
_computing_data_collection       MAR
_computing_data_reduction        MARHKL
_computing_molecular_graphics    'PLUTON [9]'
_computing_structure_refinement  'SHELXL-97 [8]'
_computing_structure_solution    'SHELXS-97 [7]'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '161 images, \D\F 3\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32314
_diffrn_reflns_theta_full        24.45
_diffrn_reflns_theta_max         24.45
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0148(15)
_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   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         6593
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+5.1418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                6063
_reflns_number_total             6593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3097.cff
_cod_data_source_block           rfdtent46
_cod_database_code               8102790