Zinc Carbodiimide Cluster Complexes: Synthesis, X-ray Crystal Structures, and Reaction Mechanism
Schmidt, Sarah; Gondzik, Sebastian; Schulz, Stephan; Bläser, Dieter; Boese, Roland; Organometallics 28 (2009) 4371–; doi:10.1021/om900373p

data_4069704
_publ_section_title
;
 Zinc Carbodiimide Cluster Complexes: Synthesis, X-ray Crystal Structures,
 and Reaction Mechanism
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4371
_journal_paper_doi               10.1021/om900373p
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety
;          
C57 H100 N8 Zn4 * 2.5 C6 H12 * 1.5 C6 H6
;
_chemical_formula_sum            'C81 H139 N8 Zn4'
_chemical_formula_weight         1486.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 115.2140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.9483(7)
_cell_length_b                   15.6718(4)
_cell_length_c                   26.9271(10)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      2.51
_cell_volume                     10670.4(6)
_computing_cell_refinement       'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER AXS SMART APEX 2 Vers. 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  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_solution    'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
; 
 Siemens SMART three axis goniometer with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2 / COSMO
;
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            63763
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 1.0-27
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3204
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.00062(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment
;
 Riding model on idealized geometrics 
 with the 1.2 fold (1.5 fold for methyl 
 groups) isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         13204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0738
_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^)+(0.1174P)^2^+53.5346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2168
_refine_ls_wR_factor_ref         0.2344
_reflns_number_gt                9719
_reflns_number_total             13204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900373p_si_001.cif
_cod_data_source_block           sar_109
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4069704