Solvent Control in the Synthesis of 3,6-Bis(pyridin-3-yl)-1,2,4,5-tetrazine-Bridged Cadmium(II) and Zinc(II) Coordination Polymers
Matthew A. Withersby; Alexander J. Blake; Neil R. Champness; Paul A. Cooke; Peter Hubberstey; Wan-Sheung Li; Martin Schröder; Inorganic Chemistry 38 (1999) 2259–2266; doi:10.1021/ic980898h

data_4321990
_publ_section_title
;
 Solvent Control in the Synthesis of
 3,6-Bis(pyridin-3-yl)-1,2,4,5-tetrazine-Bridged Cadmium(II) and Zinc(II)
 Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2259
_journal_page_last               2266
_journal_paper_doi               10.1021/ic980898h
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C18.5 H13 Cd Cl N11 O6'
_chemical_formula_weight         633.25
_chemical_name_common            {[Cd2(mu-3,3'-pytz)3(NO3)4](CH2Cl2)}n
_chemical_name_systematic
; 
 3,6-bis(pyrid-3-yl)-1,2,4,5-tetrazine Cadmium Nitrate Dichloromethane adduct 
;
_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                94.12(15)
_cell_angle_beta                 102.35(13)
_cell_angle_gamma                88.12(15)
_cell_formula_units_Z            2
_cell_length_a                   8.981(16)
_cell_length_b                   9.93(2)
_cell_length_c                   13.19(2)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      12
_cell_volume                     1146(4)
_computing_cell_refinement       'STADI-4 (stoe & cie, 1996a)'
_computing_data_collection       'STADI-4 (stoe & cie, 1996a)'
_computing_data_reduction        'X-RED (stoe & cie, 1996b)'
_computing_molecular_graphics    'SHELXTL/PC (version 5.03)(Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE STADI-4 FOUR-CIRCLE DIFFRACTOMETER'
_diffrn_measurement_method       'omega theta'
_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  0.1516
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4084
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        '+- 11.3'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Pink-Red
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Sphenoid
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.463
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.0005(6)
_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   1.041
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4031
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+10.9459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                3494
_reflns_number_total             4031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980898h_3.cif
_cod_data_source_block           cdpytz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+10.9459P] 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^)+(0.0410P)^2^+10.9459P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'geometrically placed' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_formula_sum        'C18.50 H13 Cd Cl N11 O6'
_cod_database_code               4321990