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_4069706
_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         'C46H84 N6 O Zn5 * 1.25 C5 H12'
_chemical_formula_sum            'C52.5 H103 N6 O Zn5'
_chemical_formula_weight         1161.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.978(4)
_cell_angle_beta                 108.659(3)
_cell_angle_gamma                103.379(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8446(9)
_cell_length_b                   13.7719(10)
_cell_length_c                   19.7904(13)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.36
_cell_volume                     3177.3(4)
_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(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            65125
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.896
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.65
_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    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00125(19)
_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   1.011
_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     577
_refine_ls_number_reflns         15491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+2.7454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                11685
_reflns_number_total             15491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900373p_si_001.cif
_cod_data_source_block           sarah_086
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C52.50 H103 N6 O Zn5'
_cod_database_code               4069706