Hydrogen-Bonding Network in Metal−Pterin Complexes: Synthesis and Characterization of Water-Soluble Octahedral Nickel and Cadmium Pterine Derivatives
Crispini, Alessandra; Pucci, Daniela; Bellusci, Anna; Barberio, Giovanna; La Deda, Massimo; Cataldi, Antonella; Ghedini, Mauro; Crystal Growth & Design 5 (2005) 1597–; doi:10.1021/cg050075k

data_4505128
_publ_section_title
;
 Hydrogen-Bonding Network in Metal&#x2212;Pterin Complexes:&#x2009;
 Synthesis and Characterization of Water-Soluble Octahedral Nickel and
 Cadmium Pterine Derivatives
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1597
_journal_paper_doi               10.1021/cg050075k
_journal_volume                  5
_journal_year                    2005
_chemical_formula_moiety         'C7 H13 N6 Ni0.50 O3.50'
_chemical_formula_sum            'C7 H13 N6 Ni0.5 O3.5'
_chemical_formula_weight         266.59
_chemical_name_systematic
; 
Bis(2-amino-4-hydroxypteridinate)ethylenediaminenickel(II) 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_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                 91.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8179(16)
_cell_length_b                   9.4709(19)
_cell_length_c                   15.568(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      7.78
_cell_volume                     1152.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'R3m/V Siemens'
_diffrn_measurement_method       'theta scan'
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2465
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.15
_diffrn_standards_interval_count 48
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  0.8593
_exptl_absorpt_correction_T_min  0.7407
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Linear fit to sin(theta)/lambda - 12 parameters
;
_exptl_crystal_colour            brown-yellow
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2293
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.1949
_reflns_number_gt                1650
_reflns_number_total             2293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050075ksi20050301_051021.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'C7 H13 N6 Ni0.50 O3.50'
_cod_database_code               4505128
_exptl_absorpt_factor_mur        0.226
_exptl_absorpt_correction_t_ave  0.8010
_exptl_absorpt_rmerge_before     0.0846
_exptl_absorpt_rmerge_after      0.0846