Synthesis and Structure of a Zirconium Dinitrogen Complex with a Side-On Bridging N2 Unit
Jonathan D. Cohen; Michael D. Fryzuk; Thomas M. Loehr; Murugesapillai Mylvaganam; Steven J. Rettig; Inorganic Chemistry 37 (1998) 112–119; doi:10.1021/ic9709786

data_4322597
_publ_contact_author
;
Michael D. Fryzuk
University of British Columbia
Department of Chemistry
2036 Main Mall
Vancouver, BC V6T 1Z1
Canada
;
_publ_contact_author_email       ' fryzuk@chem.ubc.ca '
_publ_contact_author_fax         ' 604-822-2847 '
_publ_contact_author_phone       ' 604-822-2897 '
_publ_section_title
;
 Synthesis and Structure of a Zirconium Dinitrogen Complex with a Side-On
 Bridging N2 Unit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              112
_journal_page_last               119
_journal_paper_doi               10.1021/ic9709786
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C52 H106 N4 O2 P4 Si4 Zr2 '
_chemical_formula_sum            'C52 H106 N4 O2 P4 Si4 Zr2'
_chemical_formula_weight         1238.11
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_date             1997-08-22
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3839(14)
_cell_length_b                   17.7539(14)
_cell_length_c                   25.9967(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      36.3
_cell_measurement_theta_min      23.2
_cell_volume                     6638.8(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.05415
_diffrn_orient_matrix_UB_12      0.02965
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_diffrn_orient_matrix_UB_22      -0.02028
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_diffrn_orient_matrix_UB_32      0.04339
_diffrn_orient_matrix_UB_33      0.00757
_diffrn_radiation_detector       'scintillation counter'
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_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6948
_diffrn_reflns_reduction_process 'Lp corrections applied'
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_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        -2.01
_diffrn_standards_interval_count 200
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_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            dark
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_exptl_crystal_density_meas      ?
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_refine_diff_density_max         0.44
_refine_diff_density_min         -0.37
_refine_ls_extinction_coef       0.000000092(5)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_obs   1.640
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
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_refine_ls_number_reflns         3444
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0370
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0340
_reflns_number_observed          3444
_reflns_number_total             6948
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            ic9709786_1.cif
_cod_data_source_block           mf182/[PNP]ZrOAr*N2
_cod_depositor_comments
;
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^(Fo)]' 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^(Fo)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6638.8(7)
_cod_original_sg_symbol_H-M      'P b c n '
_cod_original_formula_sum        'C52 H106 N4 O2 P4 Si4 Zr2 '
_cod_database_code               4322597