Reactions of a Zn(I) complex with group 14 azides ‒ formation of zinc azide and zinc hexazene complexes
S. Gondzik; S. Schulz; D. Blaser; C. Wolper; R. Haack; G. Jansena; Chem.Commun. 50 (2014) 927–; doi:10.1039/c3cc47687a

data_7110260
_publ_section_title
;
 Reactions of a Zn(I) complex with group 14 azides -- formation of zinc
 azide and zinc hexazene complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              927
_journal_paper_doi               10.1039/c3cc47687a
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C64 H72 F N10 Zn2'
_chemical_formula_weight         1131.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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-2012
_cell_angle_alpha                90
_cell_angle_beta                 104.691(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8569(9)
_cell_length_b                   17.7885(13)
_cell_length_c                   13.5948(10)
_cell_measurement_reflns_used    9552
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      32.46
_cell_measurement_theta_min      2.52
_cell_volume                     3007.6(4)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_diffrn_ambient_temperature      180(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55228
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.260
_diffrn_reflns_theta_min         1.926
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         11500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+0.9651P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8564
_reflns_number_total             11500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc47687a.txt
_cod_data_source_block           sg_510_0m
_cod_database_code               7110260
_shelx_estimated_absorpt_t_min   0.816
_shelx_estimated_absorpt_t_max   0.959
_shelxl_version_number           2012-9
_shelx_res_checksum              596
_shelx_hkl_checksum              31342