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_4077832
_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            'C50 H60 N4 O Zr'
_chemical_formula_weight         824.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.259(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.880(2)
_cell_length_b                   11.940(2)
_cell_length_c                   19.253(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      5.0
_cell_volume                     4224.5(10)
_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 0.937
_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  0.1728
_diffrn_reflns_av_sigmaI/netI    0.1596
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24863
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1993
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+3.4027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.2340
_reflns_number_gt                3071
_reflns_number_total             6996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990688s.cif
_cod_data_source_block           6
_cod_depositor_comments
;
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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4224.6(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077832