Tris[3,6-bis(2-pyridyl)pyridazine-<i>N</i>^1^,<i>N</i>^6^]nickel(II) diperchlorate 0.11-hydrate
Jau-Shuenn Wang; Chou-Fu Sheu; Jung-Si Lee; Acta Crystallographica Section C 55 (1999) 1806–1809; doi:10.1107/S0108270199009087

data_2009163
_publ_section_title
;
 Tris[3,6-bis(2-pyridyl)pyridazine-<i>N</i>^1^,<i>N</i>^6^]nickel(II)
 diperchlorate 0.11-hydrate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1806
_journal_page_last               1809
_journal_paper_doi               10.1107/S0108270199009087
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Ni (C14 H10 N4)3] 2Cl O4 , 0.11H2 O'
_chemical_formula_moiety         'C42 H30 N12 Ni, 2(Cl O4), 0.11(H2 O)'
_chemical_formula_sum            'C42 H30.22 Cl2 N12 Ni O8.11'
_chemical_formula_weight         962.43
_chemical_name_systematic
;
Tris[3,6-bis(2'-pyridyl)pyridazine-N^1^,N^6^]nickel(II) diperchlorate
0.11-hydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                81.362(10)
_cell_angle_beta                 87.180(12)
_cell_angle_gamma                67.335(9)
_cell_formula_units_Z            4
_cell_length_a                   16.249(2)
_cell_length_b                   16.3338(12)
_cell_length_c                   17.414(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      5.94
_cell_volume                     4216.3(10)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994a)'
_computing_data_reduction        'SHELXTL (Siemens, 1994b)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.020
_diffrn_reflns_av_sigmaI/netI    0.055
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15335
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        5.35
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1973
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.544
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         14748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.096
_refine_ls_R_factor_obs          .057
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0774P)^2^+4.0452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.168
_refine_ls_wR_factor_obs         .139
_reflns_number_observed          9987
_reflns_number_total             14758
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            os1057.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2018-09-25

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0774P)^2^+4.0452P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0774P)^2^+4.0452P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4216.2(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2009163