The first amidozirconium(IV)‒porphyrin complex: <i>cis</i>-[bis(trimethylsilyl)amido]chloro(tetraphenylporphyrinato)zirconium(IV)
Kim, Hee-Joon; Kim, Kimoon; Acta Crystallographica Section C 55 (1999) 1814–1815; doi:10.1107/S0108270199009919

data_2009095
_publ_section_title
;The first amidozirconium(IV)--porphyrin complex:
 <i>cis</i>-[bis(trimethylsilyl)amido]chloro(tetraphenylporphyrinato)zirconium(IV)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1814
_journal_page_last               1815
_journal_paper_doi               10.1107/S0108270199009919
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Zr Cl (C44 H28 N4) (C6 H18 N Si2)]'
_chemical_formula_sum            'C50 H46 Cl N5 Si2 Zr'
_chemical_formula_weight         899.77
_chemical_name_systematic
;
(tpp)Zr(Cl)[N(SiMe~3~)~2~]
(tpp = 5,10,15,20-tetraphenylporphyrinato dianion)
;
_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           SHELXTL
_cell_angle_alpha                99.7900(10)
_cell_angle_beta                 98.9430(10)
_cell_angle_gamma                114.3650(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9557(7)
_cell_length_b                   12.1110(7)
_cell_length_c                   17.9310(10)
_cell_measurement_reflns_used    5599
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.6
_cell_volume                     2255.8(2)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997b)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.016
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14640
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997a)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         10520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.039
_refine_ls_R_factor_gt           0.032
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0227P)^2^+1.9648P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.081
_reflns_number_gt                9504
_reflns_number_total             10520
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1353.cif
_cod_data_source_block           xc337
_cod_depositor_comments
;
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 
;
_cod_original_cell_volume        2255.9(2)
_cod_database_code               2009095
_cod_database_fobs_code          2009095