Solution and solid state coexistence of head‒head and head‒tail isomers in dimeric Pd(II) and Pt(II) complexes of the type [M2(a‒a)2(µ-L-N3N4)2]2+ with a bridging triazolopyrimidine ligand and chelating bidentate diamines
Mohammad Abul Haj; Miguel Quirós; Juan M. Salas; J. Chem. Soc., Dalton Trans.  (2002) 4740–4745; doi:10.1039/b207263g

data_1101085
_publ_section_title
;
 Solution and solid state coexistence of head--head and head--tail
 isomers in dimeric Pd(II) and Pt(II) complexes of the type
 [M2(a--a)2(&#x00B5;-L-N3N4)2]2+ with a bridging triazolopyrimidine
 ligand and chelating bidentate diamines
;
_journal_issue                   24
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4740
_journal_page_last               4745
_journal_paper_doi               10.1039/b207263g
_journal_year                    2002
_chemical_formula_sum            'C26 H29 Cl3 N16 O19 Pd2'
_chemical_formula_weight         1188.80
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1799(14)
_cell_length_b                   18.9400(18)
_cell_length_c                   9.6374(8)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      12.5
_cell_volume                     2040.7(4)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 1.05 - 1.25, scan ratio 2theta:omega = 1.00
I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3193
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        3.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.6505
_exptl_absorpt_correction_T_min  0.5388
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3193
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0821
_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^)+(0.0600P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.2107
_reflns_number_gt                1900
_reflns_number_total             3193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207263g.txt
_cod_data_source_block           compound6
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               1101085