Porphodimethene−Zirconium: A New Entry into Zirconium Macrocycle Organometallic Chemistry
Bonomo, Lucia; Toraman, Gülsen; Solari, Euro; Scopelliti, Rosario; Floriani, Carlo; Organometallics 18 (1999) 5198–; doi:10.1021/om990688s

data_4077833
_publ_section_title
;
 Porphodimethene&#x2212;Zirconium:&#x00A0; A New Entry into Zirconium
 Macrocycle Organometallic Chemistry
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5198
_journal_paper_doi               10.1021/om990688s
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C39 H53 N5 Zr'
_chemical_formula_weight         683.08
_chemical_name_systematic
; 
 ? 
;
_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                89.771(14)
_cell_angle_beta                 87.736(12)
_cell_angle_gamma                71.089(13)
_cell_formula_units_Z            2
_cell_length_a                   9.1942(8)
_cell_length_b                   10.9092(18)
_cell_length_c                   17.887(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      5.0
_cell_volume                     1695.9(4)
_computing_cell_refinement       'KUMA, CrysAlis RED, release 1.6.0'
_computing_data_collection       'KUMA, KM4CCD, release 1.5.7'
_computing_data_reduction        'KUMA, CrysAlis RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type
'KUMA 4 diffractometer equipped with a CCD detector'
_diffrn_measurement_method
'2 runs (110 frames each) using omega scan, 1 run (300 frames) using phi scan'
_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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9869
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0213P)^2^+7.8249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                4681
_reflns_number_total             5140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990688s.cif
_cod_data_source_block           9
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077833