Tris(phenanthroline)zinc dimethylazaxanthinate heptahydrate
Maldonado, Carmen R.; Quirós, Miguel; Salas, Juan M.; Personal communication to COD  (2016) –; doi:

data_3500042
_publ_section_references
;
Bruker (1999). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, 
Winsconsin, USA. 
 
Hall, S.R. & du Boulay, D. (1997). Xtal_GX. University of Western 
Australia, Perth, Australia. 
 
Sheldrick, G.M. (1997). SHELXL97. University of G\"ottingen, Germany. 
;
_publ_section_title
;
 Tris(phenanthroline)zinc dimethylazaxanthinate heptahydrate
;
_journal_name_full               'Personal communication to COD'
_journal_year                    2016
_chemical_formula_moiety         'C36 H24 N6 Zn 2+, 2(C6 H6 N5 O2 1-), 7(H2 O)'
_chemical_formula_sum            'C48 H50 N16 O11 Zn'
_chemical_formula_weight         1092.41
_chemical_name_systematic
; 
 Tris(phenanthroline)zinc dimethylazaxanthinate heptahydrate
;
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.968(1)
_cell_angle_beta                 99.884(1)
_cell_angle_gamma                113.157(1)
_cell_formula_units_Z            2
_cell_length_a                   13.8436(10)
_cell_length_b                   13.9166(10)
_cell_length_c                   15.0218(11)
_cell_measurement_reflns_used    7256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.2
_cell_volume                     2426.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28529
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        -0.1
_diffrn_standards_number         558
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.42
_exptl_special_details
; 
 ? 
;
_geom_special_details
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         10992
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0600P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1333
_refine_special_details
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_reflns_number_gt                10289
_reflns_number_total             10992
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            znf3ax.cif
_cod_data_source_block           znf3ax
_cod_database_code               3500042
_cod_database_fobs_code          3500042