Molecular Structures of Ge(tpp)(OAc)2and In(tpp)(OAc) and Their Implications: Correlations between the 13C NMR Chemical Shift of the Acetato Ligand and Different Types of Carboxylate Coordination in M(por)(OAc)n {por = tpp (5,10,15,20-Tetraphenylporphyrinate), tmpp (5,10,15,20-Tetrakis(4-methoxyphenyl)porphyrinate), tpyp (5,10,15,20-Tetrakis(4-pyridyl)porphyrinate); M = Ga, In, Tl, Ge, Sn; n= 1, 2}
Shwu-Juian Lin; Tay-Ning Hong; Jo-Yu Tung; Jyh-Horung Chen; Inorganic Chemistry 36 (1997) 3886–3891; doi:10.1021/ic961304i

data_4323556
_publ_section_title
;
 Molecular Structures of Ge(tpp)(OAc)2and In(tpp)(OAc) and Their
 Implications: Correlations between the 13C NMR Chemical Shift of the
 Acetato Ligand and Different Types of Carboxylate Coordination in
 M(por)(OAc)n {por = tpp (5,10,15,20-Tetraphenylporphyrinate), tmpp
 (5,10,15,20-Tetrakis(4-methoxyphenyl)porphyrinate), tpyp
 (5,10,15,20-Tetrakis(4-pyridyl)porphyrinate); M = Ga, In, Tl, Ge, Sn; n=
 1, 2}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3886
_journal_page_last               3891
_journal_paper_doi               10.1021/ic961304i
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'C48H34GeN4O4 (CH2Cl2)2'
_chemical_formula_sum            'C50 H38 Cl4 Ge N4 O4'
_chemical_formula_weight         973.2
_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_type_scat_source           'International Table vol IV'
_cell_angle_alpha                61.52(1)
_cell_angle_beta                 74.50(1)
_cell_angle_gamma                74.30(1)
_cell_formula_units_Z            1
_cell_length_a                   10.167(2)
_cell_length_b                   11.358(2)
_cell_length_c                   11.672(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2
_cell_volume                     1125.2(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_measurement_device       'Siemens R 3m/V diffractometer'
_diffrn_measurement_method       2\q-\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5176
_diffrn_reflns_theta_max         14
_diffrn_standards_decay_%        26
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.40
_refine_diff_density_min         -0.70
_refine_ls_extinction_coef       None
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.29
_refine_ls_hydrogen_treatment    'Riding model, fixed isotropic U'
_refine_ls_number_parameters     304
_refine_ls_number_reflns         2895
_refine_ls_R_factor_obs          0.077
_refine_ls_shift/esd_max         0.035
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+0.0030F^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.098
_reflns_number_observed          2895
_reflns_number_total             4909
_reflns_observed_criterion       F>4.0\s(F)
_cod_data_source_file            ic961304i_1.cif
_cod_data_source_block           (I)_Ge(tpp)(OAc)2.2CH2Cl2
_cod_depositor_comments
;
 Adding the coordinates and the atom displacement parameter values
 for the hydrogen atoms from the supplementary material of the
 original publication.

 Antanas Vaitkus,
 2017-01-05

 Marking atoms 'C(21)', 'O(2)' and 'C(21')', 'O(2')' as belonging
 to two disordered groups with the occupancy of 0.5 each after
 consulting the original publication.

 Antanas Vaitkus,
 2017-01-05

 Adding a missing closing parenthesis (')') to the _geom_angle
 data item value '118.0(10' after consulting the original
 publication.

 Antanas Vaitkus,
 2017-01-05

 Adding missing minus signs ('-') to the _atom_site_aniso_U_*,
 _atom_site_fract_* data item values.

 Antanas Vaitkus,
 2017-01-05

 Correcting typos in the _atom_site_label, _atom_site_aniso_label,
 _geom_angle_atom_site_label_*, _geom_bond_atom_site_label_* data item values.

 Antanas Vaitkus,
 2017-01-05

 Correcting a typo in the _atom_site_label data item value by changing it
 from 'C1(2)' to 'Cl(2)'. Related data items (e. g. _atom_site_aniso_label)
 were also changed accordingly.

 Antanas Vaitkus,
 2017-01-05

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 'w^-1^=\s^2^(F)+0.0030F^2^' 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^(F)+0.0030F^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1125.2(5)
_cod_database_code               4323556