#------------------------------------------------------------------------------
#$Date: 2015-10-09 11:24:57 +0300 (Fri, 09 Oct 2015) $
#$Revision: 161279 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/60/7036069.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_7036069
loop_
_publ_author_name
'Gondzik, S.'
'Wölper, C'
'Haack, R.'
'Jansen, G.'
'Schulz, S.'
_publ_section_title
;
 (Me)L2Zn2(μ-1,6-Ph2-N6) - a building block for new hexazene complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15703
_journal_page_last               15711
_journal_paper_doi               10.1039/c5dt02423d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C30 H34 N8 Zn2'
_chemical_formula_weight         637.39
_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-2014/7
_audit_update_record
;
2015-06-22 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.059(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0346(5)
_cell_length_b                   16.9894(8)
_cell_length_c                   10.1868(5)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      33.06
_cell_measurement_theta_min      2.36
_cell_volume                     1546.57(13)
_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 0.994
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            44303
_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         2.362
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.62
_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            orange
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.156
_refine_diff_density_max         1.566
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         5932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0372
_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/[σ²(Fo²)+(0.0628P)²+0.3516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4851
_reflns_number_total             5932
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02423d2.cif
_cod_data_source_block           sg670m
_cod_depositor_comments
'Adding full bibliography for 7036068--7036069.cif.'
_cod_database_code               7036069
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.611
_shelx_estimated_absorpt_t_max   0.790
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Zn1 Zn 0.97389(2) 0.07069(2) 0.78560(2) 0.01790(6) Uani 1 1 d . .
N1 N 0.84763(13) 0.10315(7) 0.88639(12) 0.0166(2) Uani 1 1 d . .
N2 N 0.86068(13) 0.05983(7) 0.99806(13) 0.0176(2) Uani 1 1 d . .
N3 N 0.95900(13) 0.00370(7) 1.03998(12) 0.0178(2) Uani 1 1 d . .
N4 N 0.81657(16) -0.01066(8) 0.63425(14) 0.0269(3) Uani 1 1 d . .
C1 C 0.73726(14) 0.16241(8) 0.84700(14) 0.0171(2) Uani 1 1 d . .
C2 C 0.64984(16) 0.17534(9) 0.92013(16) 0.0209(3) Uani 1 1 d . .
H2 H 0.6636 0.1437 1.0023 0.025 Uiso 1 1 calc R U
C3 C 0.54300(17) 0.23471(9) 0.87161(16) 0.0252(3) Uani 1 1 d . .
H3 H 0.4836 0.2431 0.9211 0.030 Uiso 1 1 calc R U
C4 C 0.52108(17) 0.28225(9) 0.75193(18) 0.0257(3) Uani 1 1 d . .
H4 H 0.4480 0.3229 0.7202 0.031 Uiso 1 1 calc R U
C5 C 0.60745(17) 0.26935(9) 0.68008(17) 0.0243(3) Uani 1 1 d . .
H5 H 0.5933 0.3012 0.5981 0.029 Uiso 1 1 calc R U
C6 C 0.71495(15) 0.21011(9) 0.72669(16) 0.0212(2) Uani 1 1 d . .
H6 H 0.7737 0.2020 0.6765 0.025 Uiso 1 1 calc R U
C7 C 1.08518(19) 0.12987(10) 0.70233(19) 0.0283(3) Uani 1 1 d . .
H7A H 1.0947 0.0979 0.6269 0.042 Uiso 1 1 calc R U
H7B H 1.1850 0.1426 0.7807 0.042 Uiso 1 1 calc R U
H7C H 1.0315 0.1786 0.6577 0.042 Uiso 1 1 calc R U
C8 C 0.73925(19) -0.05883(10) 0.56180(17) 0.0251(3) Uani 1 1 d . .
C9 C 0.6414(2) -0.12096(11) 0.47007(19) 0.0339(4) Uani 1 1 d . .
H9A H 0.5375 -0.1083 0.4455 0.051 Uiso 1 1 calc R U
H9B H 0.6693 -0.1710 0.5237 0.051 Uiso 1 1 calc R U
H9C H 0.6517 -0.1255 0.3792 0.051 Uiso 1 1 calc R U
C10 C 0.6928(2) 0.14835(13) 0.3453(2) 0.0400(4) Uani 1 1 d . .
H10 H 0.7648 0.1852 0.4079 0.048 Uiso 1 1 calc R U
C11 C 0.5423(2) 0.16271(12) 0.2968(2) 0.0405(4) Uani 1 1 d . .
H11 H 0.5107 0.2095 0.3255 0.049 Uiso 1 1 calc R U
C12 C 0.4379(2) 0.10865(13) 0.2062(2) 0.0395(4) Uani 1 1 d . .
H12 H 0.3342 0.1180 0.1735 0.047 Uiso 1 1 calc R U
C13 C 0.4842(2) 0.04102(13) 0.1634(2) 0.0376(4) Uani 1 1 d . .
H13 H 0.4124 0.0041 0.1007 0.045 Uiso 1 1 calc R U
C14 C 0.6345(2) 0.02721(12) 0.2117(2) 0.0376(4) Uani 1 1 d . .
H14 H 0.6663 -0.0192 0.1820 0.045 Uiso 1 1 calc R U
C15 C 0.7389(2) 0.08057(13) 0.3032(2) 0.0376(4) Uani 1 1 d . .
H15 H 0.8426 0.0707 0.3372 0.045 Uiso 1 1 calc R U
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C7 Zn1 N3 132.15(6) . 3_757
C7 Zn1 N1 133.41(6) . .
N3 Zn1 N1 76.23(4) 3_757 .
C7 Zn1 N4 113.52(7) . .
N3 Zn1 N4 94.06(5) 3_757 .
N1 Zn1 N4 96.55(5) . .
N2 N1 C1 113.74(11) . .
N2 N1 Zn1 116.50(9) . .
C1 N1 Zn1 129.55(9) . .
N3 N2 N1 117.35(11) . .
N2 N3 N3 115.74(13) . 3_757
N2 N3 Zn1 130.24(9) . 3_757
N3 N3 Zn1 113.82(11) 3_757 3_757
C8 N4 Zn1 174.27(14) . .
C6 C1 C2 119.01(12) . .
C6 C1 N1 116.97(12) . .
C2 C1 N1 124.02(12) . .
C3 C2 C1 119.52(13) . .
C2 C3 C4 121.41(14) . .
C5 C4 C3 118.92(13) . .
C4 C5 C6 120.62(14) . .
C5 C6 C1 120.52(13) . .
N4 C8 C9 179.4(2) . .
C11 C10 C15 120.21(19) . .
C10 C11 C12 119.68(19) . .
C13 C12 C11 120.06(18) . .
C14 C13 C12 119.97(19) . .
C13 C14 C15 120.11(18) . .
C14 C15 C10 119.97(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 C7 1.9594(15) .
Zn1 N3 2.0297(11) 3_757
Zn1 N1 2.0365(11) .
Zn1 N4 2.1366(14) .
N1 N2 1.3104(16) .
N1 C1 1.4132(17) .
N2 N3 1.2968(16) .
N3 N3 1.402(2) 3_757
N3 Zn1 2.0297(11) 3_757
N4 C8 1.138(2) .
C1 C6 1.3998(19) .
C1 C2 1.4025(19) .
C2 C3 1.389(2) .
C3 C4 1.394(2) .
C4 C5 1.383(2) .
C5 C6 1.391(2) .
C8 C9 1.455(2) .
C10 C11 1.380(3) .
C10 C15 1.380(3) .
C11 C12 1.383(3) .
C12 C13 1.382(3) .
C13 C14 1.378(3) .
C14 C15 1.378(3) .
