#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:23:31 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178562 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/71/4067157.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4067157
loop_
_publ_author_name
'Schmidt, Sarah'
'Schulz, Stephan'
'Bläser, Dieter'
'Boese, Roland'
'Bolte, Michael'
_publ_section_title
;
 Synthesis and Structural Characterization of New Zinc Amidinate Complexes
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6097
_journal_paper_doi               10.1021/om1008549
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C30 H46 N2 Zn'
_chemical_formula_weight         500.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.911(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5876(4)
_cell_length_b                   16.9607(8)
_cell_length_c                   17.9403(8)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.34
_cell_volume                     2831.8(2)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA 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 D8 KAPPA APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.994
_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  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29178
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.67
_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            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0262
_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/[σ²(Fo²)+(0.0360P)²+1.3402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                5563
_reflns_number_total             6459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1008549_si_003.cif
_cod_data_source_block           sar_260m_CCDC-785893_(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4067157
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.313224(16) 0.178064(9) 0.218812(8) 0.01589(5) Uani 1 1 d .
N1 N 0.28723(11) 0.17997(6) 0.32094(6) 0.0131(2) Uani 1 1 d .
N2 N 0.14531(11) 0.06719(6) 0.29860(6) 0.0143(2) Uani 1 1 d .
C1 C 0.20671(13) 0.12254(7) 0.34479(7) 0.0130(2) Uani 1 1 d .
C2 C 0.16731(14) 0.06197(8) 0.22432(8) 0.0153(3) Uani 1 1 d .
C3 C 0.28429(14) 0.01583(8) 0.21238(8) 0.0178(3) Uani 1 1 d .
C4 C 0.29366(16) 0.00074(9) 0.13760(9) 0.0236(3) Uani 1 1 d .
H4 H 0.3716 -0.0308 0.1291 0.028 Uiso 1 1 d R
C5 C 0.19238(17) 0.03037(9) 0.07515(8) 0.0266(3) Uani 1 1 d .
H5 H 0.1991 0.0182 0.0239 0.032 Uiso 1 1 d R
C6 C 0.08207(17) 0.07728(9) 0.08678(8) 0.0243(3) Uani 1 1 d .
H6 H 0.0133 0.0981 0.0432 0.029 Uiso 1 1 d R
C7 C 0.06808(15) 0.09518(8) 0.16058(8) 0.0187(3) Uani 1 1 d .
C8 C 0.38952(14) -0.02036(8) 0.28092(8) 0.0202(3) Uani 1 1 d .
H8 H 0.3978 0.0153 0.3233 0.024 Uiso 1 1 d R
C9 C 0.33061(18) -0.09835(9) 0.30355(10) 0.0295(3) Uani 1 1 d .
H9A H 0.2359 -0.0896 0.3138 0.044 Uiso 1 1 d R
H9B H 0.3964 -0.1193 0.3498 0.044 Uiso 1 1 d R
H9C H 0.3219 -0.1362 0.2614 0.044 Uiso 1 1 d R
C10 C 0.54001(17) -0.03174(12) 0.26817(11) 0.0370(4) Uani 1 1 d .
H10A H 0.5370 -0.0727 0.2293 0.055 Uiso 1 1 d R
H10B H 0.6061 -0.0478 0.3164 0.055 Uiso 1 1 d R
H10C H 0.5734 0.0178 0.2504 0.055 Uiso 1 1 d R
C11 C -0.05625(15) 0.14509(8) 0.17239(8) 0.0222(3) Uani 1 1 d .
H11 H -0.0336 0.1623 0.2249 0.027 Uiso 1 1 d R
C12 C -0.19363(18) 0.09607(10) 0.15889(12) 0.0355(4) Uani 1 1 d .
H12A H -0.2194 0.0785 0.1053 0.053 Uiso 1 1 d R
H12B H -0.2718 0.1281 0.1694 0.053 Uiso 1 1 d R
H12C H -0.1778 0.0501 0.1929 0.053 Uiso 1 1 d R
C13 C -0.08073(19) 0.21805(10) 0.12138(11) 0.0361(4) Uani 1 1 d .
H13A H 0.0083 0.2487 0.1299 0.054 Uiso 1 1 d R
H13B H -0.1566 0.2505 0.1339 0.054 Uiso 1 1 d R
H13C H -0.1097 0.2018 0.0675 0.054 Uiso 1 1 d R
C14 C 0.35527(13) 0.24528(7) 0.36673(7) 0.0137(2) Uani 1 1 d .
C15 C 0.27838(14) 0.31586(8) 0.36836(8) 0.0162(3) Uani 1 1 d .
C16 C 0.34742(15) 0.37853(8) 0.41248(8) 0.0198(3) Uani 1 1 d .
H16 H 0.2954 0.4265 0.4146 0.024 Uiso 1 1 d R
C17 C 0.48930(15) 0.37312(8) 0.45310(8) 0.0204(3) Uani 1 1 d .
H17 H 0.5338 0.4159 0.4852 0.025 Uiso 1 1 d R
C18 C 0.56649(15) 0.30561(8) 0.44702(8) 0.0200(3) Uani 1 1 d .
H18 H 0.6661 0.3029 0.4734 0.024 Uiso 1 1 d R
C19 C 0.50289(14) 0.24123(8) 0.40357(8) 0.0161(3) Uani 1 1 d .
C20 C 0.12543(14) 0.32630(8) 0.32058(8) 0.0187(3) Uani 1 1 d .
H20 H 0.0845 0.2749 0.3083 0.022 Uiso 1 1 d R
C21 C 0.12862(16) 0.36806(10) 0.24505(9) 0.0256(3) Uani 1 1 d .
H21A H 0.1705 0.4207 0.2564 0.038 Uiso 1 1 d R
H21B H 0.0306 0.3729 0.2131 0.038 Uiso 1 1 d R
H21C H 0.1870 0.3374 0.2175 0.038 Uiso 1 1 d R
C22 C 0.02847(16) 0.37213(9) 0.36207(9) 0.0252(3) Uani 1 1 d .
H22A H 0.0354 0.3489 0.4129 0.038 Uiso 1 1 d R
H22B H -0.0713 0.3695 0.3319 0.038 Uiso 1 1 d R
H22C H 0.0596 0.4273 0.3679 0.038 Uiso 1 1 d R
C23 C 0.59484(14) 0.17090(8) 0.39369(8) 0.0194(3) Uani 1 1 d .
H23 H 0.5315 0.1277 0.3747 0.023 Uiso 1 1 d R
C24 C 0.69921(16) 0.14383(9) 0.46791(9) 0.0255(3) Uani 1 1 d .
H24A H 0.7728 0.1844 0.4849 0.038 Uiso 1 1 d R
H24B H 0.7452 0.0944 0.4586 0.038 Uiso 1 1 d R
H24C H 0.6464 0.1355 0.5077 0.038 Uiso 1 1 d R
C25 C 0.67954(17) 0.19003(10) 0.33322(9) 0.0282(3) Uani 1 1 d .
H25A H 0.6125 0.2035 0.2845 0.042 Uiso 1 1 d R
H25B H 0.7367 0.1440 0.3259 0.042 Uiso 1 1 d R
H25C H 0.7436 0.2348 0.3508 0.042 Uiso 1 1 d R
C26 C 0.38445(17) 0.21777(10) 0.13415(9) 0.0270(3) Uani 1 1 d .
H26A H 0.3481 0.2713 0.1214 0.041 Uiso 1 1 d R
H26B H 0.3517 0.1834 0.0894 0.041 Uiso 1 1 d R
H26C H 0.4897 0.2187 0.1486 0.041 Uiso 1 1 d R
C27 C 0.18726(14) 0.11542(8) 0.42748(8) 0.0164(3) Uani 1 1 d .
C28 C 0.11492(16) 0.18768(9) 0.45325(8) 0.0221(3) Uani 1 1 d .
H28A H 0.0251 0.1991 0.4153 0.033 Uiso 1 1 d R
H28B H 0.1794 0.2332 0.4577 0.033 Uiso 1 1 d R
H28C H 0.0942 0.1770 0.5032 0.033 Uiso 1 1 d R
C29 C 0.33379(15) 0.10150(9) 0.48370(8) 0.0225(3) Uani 1 1 d .
H29A H 0.3195 0.0885 0.5346 0.034 Uiso 1 1 d R
H29B H 0.3923 0.1493 0.4872 0.034 Uiso 1 1 d R
H29C H 0.3830 0.0578 0.4651 0.034 Uiso 1 1 d R
C30 C 0.09221(17) 0.04405(9) 0.43268(9) 0.0252(3) Uani 1 1 d .
H30A H 0.0825 0.0384 0.4856 0.038 Uiso 1 1 d R
H30B H 0.1365 -0.0036 0.4177 0.038 Uiso 1 1 d R
H30C H -0.0030 0.0516 0.3982 0.038 Uiso 1 1 d R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 Zn1 C26 154.48(6)
N1 Zn1 C2 76.43(4)
C26 Zn1 C2 129.09(6)
C1 N1 C14 125.43(11)
C1 N1 Zn1 120.01(9)
C14 N1 Zn1 114.55(8)
C1 N2 C2 120.31(11)
N2 C1 N1 121.16(12)
N2 C1 C27 114.62(11)
N1 C1 C27 124.16(11)
N2 C2 C7 121.14(12)
N2 C2 C3 118.78(12)
C7 C2 C3 119.80(12)
N2 C2 Zn1 101.96(8)
C7 C2 Zn1 85.78(8)
C3 C2 Zn1 87.55(8)
C4 C3 C2 118.82(13)
C4 C3 C8 121.48(13)
C2 C3 C8 119.56(12)
C5 C4 C3 121.15(14)
C6 C5 C4 120.00(14)
C5 C6 C7 121.40(14)
C6 C7 C2 118.70(13)
C6 C7 C11 120.76(13)
C2 C7 C11 120.44(12)
C3 C8 C10 113.41(13)
C3 C8 C9 110.36(12)
C10 C8 C9 110.65(13)
C7 C11 C13 112.46(13)
C7 C11 C12 110.52(12)
C13 C11 C12 110.15(13)
C15 C14 C19 120.11(12)
C15 C14 N1 119.87(11)
C19 C14 N1 119.70(11)
C16 C15 C14 118.68(12)
C16 C15 C20 119.56(12)
C14 C15 C20 121.70(12)
C17 C16 C15 121.41(13)
C18 C17 C16 119.40(13)
C17 C18 C19 121.51(13)
C18 C19 C14 118.56(12)
C18 C19 C23 119.49(12)
C14 C19 C23 121.87(12)
C15 C20 C22 113.58(12)
C15 C20 C21 109.27(11)
C22 C20 C21 109.71(12)
C19 C23 C24 114.23(12)
C19 C23 C25 109.66(12)
C24 C23 C25 109.34(12)
C30 C27 C28 107.13(11)
C30 C27 C29 107.56(11)
C28 C27 C29 109.45(12)
C30 C27 C1 109.36(11)
C28 C27 C1 113.28(11)
C29 C27 C1 109.87(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Zn1 N1 1.9077(11)
Zn1 C26 1.9302(14)
Zn1 C2 2.4311(12)
N1 C1 1.3736(16)
N1 C14 1.4387(16)
N2 C1 1.2961(17)
N2 C2 1.4011(17)
C1 C27 1.5438(18)
C2 C7 1.4166(19)
C2 C3 1.4254(19)
C3 C4 1.390(2)
C3 C8 1.5199(19)
C4 C5 1.388(2)
C5 C6 1.379(2)
C6 C7 1.396(2)
C7 C11 1.518(2)
C8 C10 1.526(2)
C8 C9 1.531(2)
C11 C13 1.523(2)
C11 C12 1.527(2)
C14 C15 1.4098(18)
C14 C19 1.4124(18)
C15 C16 1.3938(19)
C15 C20 1.5206(18)
C16 C17 1.383(2)
C17 C18 1.382(2)
C18 C19 1.3939(19)
C19 C23 1.5187(19)
C20 C22 1.5346(19)
C20 C21 1.536(2)
C23 C24 1.5312(19)
C23 C25 1.538(2)
C27 C30 1.5315(18)
C27 C28 1.5333(19)
C27 C29 1.5380(19)
