Zircona-phosphazine complexes: synthesis and X-ray determination
Cadierno, Victorio; Zablocka, Maria; Donnadieu, Bruno; Igau, Alain; Majoral, Jean-Pierre; New Journal of Chemistry 27 (2003) 675–; doi:10.1039/b210773m

data_7050501
_publ_section_title
;
 Zircona-phosphazine complexes: synthesis and X-ray determination
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              675
_journal_paper_doi               10.1039/b210773m
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C34 H31 N2 O2 P Zr'
_chemical_formula_weight         621.80
_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                 107.921(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.125(2)
_cell_length_b                   7.8428(9)
_cell_length_c                   19.805(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_volume                     2826.5(6)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18630
_diffrn_reflns_theta_full        24.19
_diffrn_reflns_theta_max         24.19
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.6538P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0601
_reflns_number_gt                3833
_reflns_number_total             4443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210773m.txt
_cod_data_source_block           (3a)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_original_cell_volume        2826.4(5)
_cod_original_sg_symbol_H-M      ' P 21/n'
_cod_database_code               7050501
_cell_measurement_2theta_min     4.3
_cell_measurement_2theta_max     48.2
_computing_corr_abs              DIFABS