The square-pyramidal Pd^II^ complex of a cross-bridged tetraazamacrocycle
Hubin, Timothy J.; Alcock, Nathaniel W.; Busch, Daryle H.; Acta Crystallographica Section C 55 (1999) 1404–1406; doi:10.1107/S0108270199007817

data_2008879
_publ_section_title
;
 The square-pyramidal Pd^II^ complex of a cross-bridged
 tetraazamacrocycle
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1404
_journal_page_last               1406
_journal_paper_doi               10.1107/S0108270199007817
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[PdCl(C14 H30 N4 )]Cl , 2H2 0'
_chemical_formula_moiety         '[PdCl(C14 H30 N4 )]Cl , 2H2 0'
_chemical_formula_sum            'C14 H34 Cl2 N4 O2 Pd'
_chemical_formula_weight         467.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.3920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.7207(13)
_cell_length_b                   7.7934(3)
_cell_length_c                   17.2154(7)
_cell_measurement_reflns_used    5706
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3894.6(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      188(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measurement_device_type
' Siemens SMART diffractometer with Cryostream cooler (Cosier & Glazer, 1986)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11454
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.945
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0888
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                3177
_reflns_number_total             4583
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            cf1310.cif
_cod_data_source_block           timpd4
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-08-07

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

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

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 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (5
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0420P)^2^] 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^)+(0.0420P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2008879
_cod_database_fobs_code          2008879