#------------------------------------------------------------------------------
#$Date: 2015-10-09 11:24:57 +0300 (Fri, 09 Oct 2015) $
#$Revision: 161279 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/60/7036068.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_7036068
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            'C20 H16 D6 N6 Zn2'
_chemical_formula_weight         483.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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-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                 99.501(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0073(16)
_cell_length_b                   12.6894(10)
_cell_length_c                   7.7367(6)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      33.09
_cell_measurement_theta_min      3.13
_cell_volume                     2034.1(3)
_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 0.970
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.279
_diffrn_reflns_theta_min         1.882
_exptl_absorpt_coefficient_mu    2.376
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 TWINABS - Bruker AXS scaling for twinned crystals - Version 2008/4
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         3744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0381
_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)+(0.0320P)²+9.3953P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3341
_reflns_number_total             3744
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02423d2.cif
_cod_data_source_block           sg_626bm_twin5
_cod_depositor_comments
'Adding full bibliography for 7036068--7036069.cif.'
_cod_database_code               7036068
_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   0.435
_shelx_estimated_absorpt_t_max   0.764
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.42944(2) 0.36903(2) 0.10380(5) 0.01339(7) Uani 1 1 d . .
N1 N 0.39307(11) 0.47124(19) -0.0909(3) 0.0135(4) Uani 1 1 d . .
N2 N 0.43329(11) 0.53761(16) -0.1437(3) 0.0115(4) Uani 1 1 d . .
N3 N 0.49301(11) 0.53682(18) -0.0658(3) 0.0125(4) Uani 1 1 d . .
C1 C 0.32922(13) 0.4797(2) -0.1858(4) 0.0155(5) Uani 1 1 d . .
C2 C 0.29501(16) 0.3877(3) -0.2276(6) 0.0288(7) Uani 1 1 d . .
H2 H 0.3143 0.3216 -0.1934 0.035 Uiso 1 1 calc R U
C3 C 0.23232(18) 0.3919(3) -0.3197(6) 0.0327(8) Uani 1 1 d . .
H3 H 0.2092 0.3285 -0.3505 0.039 Uiso 1 1 calc R U
C4 C 0.20346(16) 0.4881(3) -0.3667(5) 0.0277(7) Uani 1 1 d . .
H4 H 0.1605 0.4909 -0.4283 0.033 Uiso 1 1 calc R U
C5 C 0.23754(17) 0.5798(3) -0.3235(5) 0.0284(7) Uani 1 1 d . .
H5 H 0.2180 0.6459 -0.3566 0.034 Uiso 1 1 calc R U
C6 C 0.30080(14) 0.5761(2) -0.2312(6) 0.0235(6) Uani 1 1 d . .
H6 H 0.3240 0.6395 -0.2000 0.028 Uiso 1 1 calc R U
C7 C 0.41603(15) 0.2192(2) 0.1436(4) 0.0198(6) Uani 1 1 d . .
H7A H 0.3699 0.2030 0.1157 0.030 Uiso 1 1 calc R U
H7B H 0.4319 0.2022 0.2667 0.030 Uiso 1 1 calc R U
H7C H 0.4396 0.1774 0.0684 0.030 Uiso 1 1 calc R U
C91 C 0.4685(3) 0.9243(3) 0.2129(7) 0.0438(11) Uani 1 1 d . .
D91 D 0.4467 0.9895 0.1877 0.053 Uiso 1 1 calc R U
C92 C 0.4350(3) 0.8298(4) 0.1726(5) 0.0436(10) Uani 1 1 d . .
D92 D 0.3908 0.8299 0.1198 0.052 Uiso 1 1 calc R U
C93 C 0.4681(3) 0.7359(3) 0.2119(6) 0.0425(11) Uani 1 1 d . .
D93 D 0.4464 0.6708 0.1857 0.051 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'
D D 0.0000 0.0000 '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 N1 133.58(12) . .
C7 Zn1 N3 135.89(11) . 5_665
N1 Zn1 N3 74.75(9) . 5_665
C7 Zn1 N2 110.91(11) . 6_566
N1 Zn1 N2 105.02(9) . 6_566
N3 Zn1 N2 84.52(9) 5_665 6_566
N2 N1 C1 113.2(2) . .
N2 N1 Zn1 117.30(18) . .
C1 N1 Zn1 129.48(18) . .
N3 N2 N1 118.4(2) . .
N3 N2 Zn1 107.26(15) . 6_565
N1 N2 Zn1 132.19(18) . 6_565
N2 N3 N3 114.8(3) . 5_665
N2 N3 Zn1 130.49(17) . 5_665
N3 N3 Zn1 114.7(2) 5_665 5_665
C2 C1 C6 120.2(3) . .
C2 C1 N1 117.8(3) . .
C6 C1 N1 121.9(3) . .
C1 C2 C3 120.0(3) . .
C4 C3 C2 120.3(4) . .
C5 C4 C3 119.6(3) . .
C4 C5 C6 120.4(3) . .
C1 C6 C5 119.5(3) . .
C91 C91 C92 121.0(3) 2_655 .
C93 C92 C91 118.1(5) . .
C93 C93 C92 120.9(3) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 C7 1.953(3) .
Zn1 N1 2.038(2) .
Zn1 N3 2.080(2) 5_665
Zn1 N2 2.275(2) 6_566
N1 N2 1.305(3) .
N1 C1 1.423(4) .
N2 N3 1.299(3) .
N2 Zn1 2.275(2) 6_565
N3 N3 1.378(5) 5_665
N3 Zn1 2.080(2) 5_665
C1 C2 1.381(4) .
C1 C6 1.381(4) .
C2 C3 1.391(5) .
C3 C4 1.385(6) .
C4 C5 1.378(5) .
C5 C6 1.402(5) .
C91 C91 1.351(11) 2_655
C91 C92 1.400(7) .
C92 C93 1.388(7) .
C93 C93 1.371(11) 2_655
