(MeZn)2(μ-η2:η2-N6Ph2): A Powerful Starting Reagent for the Synthesis of Metal Hexazene Complexes
Stienen, Christian; Gondzik, Sebastian; Gehlhaar, Alexander; Haack, Rebekka; Wölper, Christoph; Jansen, Georg; Schulz, Stephan; Organometallics 35 (2016) 1022–; doi:10.1021/acs.organomet.6b00116

data_4088469
_publ_contact_author
;
         Prof. Dr. Schulz, Stephan
         Fachbereich Chemie der
         Universit\"at Duisburg-Essen
         Campus Essen, Universit\"atsstr. 7
         D-45141 Essen, Germany
;
_publ_section_title
;
 (MeZn)2(\m-\h2:\h2-N6Ph2): A Powerful Starting Reagent for the Synthesis
 of Metal Hexazene Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1022
_journal_paper_doi               10.1021/acs.organomet.6b00116
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C46 H44 N10 Zn2'
_chemical_formula_weight         867.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                101.272(3)
_cell_angle_beta                 105.138(2)
_cell_angle_gamma                95.015(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9002(4)
_cell_length_b                   10.8554(6)
_cell_length_c                   11.3702(6)
_cell_measurement_reflns_used    9087
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.93
_cell_measurement_theta_min      2.38
_cell_volume                     1028.78(9)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.909
_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  0.0255
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            56655
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.310
_diffrn_reflns_theta_min         1.934
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 TWINABS - Bruker AXS scaling for twinned crystals - Version 2008/4
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       prism
_exptl_crystal_F_000             450
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         7229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.2508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6398
_reflns_number_total             7229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00116_si_002.cif
_cod_data_source_block           chs_088_tw4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4088469
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.900
_shelx_res_checksum              8368
_shelx_hkl_checksum              1895