#------------------------------------------------------------------------------
#$Date: 2017-01-07 17:15:11 +0200 (Sat, 07 Jan 2017) $
#$Revision: 190011 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/48/7114893.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_7114893
loop_
_publ_author_name
'Hao, Haijun'
'Cui, Chunming'
'Roesky, Herbert W.'
'Bai, Guangcai'
'Schmidt, Hans-Georg'
'Noltemeyer, Mathias'
_publ_section_title
;
 Syntheses and structures of the first examples of zinc compounds with
 bridging fluorine and hydrogen atoms
;
_journal_issue                   12
_journal_name_full               'Chemical Communications'
_journal_page_first              1118
_journal_paper_doi               10.1039/b102275j
_journal_year                    2001
_chemical_formula_sum            'C48 H58 N4 Zn2'
_chemical_formula_weight         821.72
_chemical_name_systematic        ?
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.941(5)
_cell_length_b                   20.576(3)
_cell_length_c                   24.918(4)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     8686(3)
_computing_cell_refinement       'STOE DIF4'
_computing_data_collection       'STOE DIF4'
_computing_data_reduction        'STOE REDU4'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE AED2 four circle diffractometer'
_diffrn_measurement_method       'profile fitted theta omega scans'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            3065
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.5993
_exptl_absorpt_correction_T_min  0.4622
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0374P)²+20.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                1699
_reflns_number_total             1915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102275j.txt
_cod_data_source_block           roe909b
_cod_original_sg_symbol_H-M      Fddd
_cod_original_formula_sum        'C48 H58 N4 Zn2 incl. benzene'
_cod_database_code               7114893
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C48 H58 N4 Zn2 be cl e en in nz' to 'C48 H58 N4 Zn2'.

 Antanas Vaitkus,
 2017-01-07
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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 0.197348(19) 0.1250 0.1250 0.02578(14) Uani 1 2 d S
N1 N 0.27320(10) 0.19385(8) 0.14347(7) 0.0243(4) Uani 1 1 d .
C1 C 0.35086(12) 0.18319(10) 0.14207(8) 0.0259(4) Uani 1 1 d .
C2 C 0.38574(17) 0.1250 0.1250 0.0280(6) Uani 1 2 d S
H2A H 0.4418 0.1250 0.1250 0.034 Uiso 1 2 calc SR
C3 C 0.40620(14) 0.23651(12) 0.15985(10) 0.0374(5) Uani 1 1 d .
H3A H 0.3980 0.2751 0.1374 0.056 Uiso 1 1 calc R
H3B H 0.4609 0.2217 0.1562 0.056 Uiso 1 1 calc R
H3C H 0.3956 0.2474 0.1974 0.056 Uiso 1 1 calc R
C11 C 0.24722(12) 0.25689(10) 0.16031(8) 0.0249(4) Uani 1 1 d .
C12 C 0.23945(13) 0.30642(11) 0.12205(9) 0.0312(5) Uani 1 1 d .
C13 C 0.21930(16) 0.36831(12) 0.13938(10) 0.0393(6) Uani 1 1 d .
H13A H 0.2157 0.4027 0.1140 0.047 Uiso 1 1 calc R
C14 C 0.20440(15) 0.38074(12) 0.19274(11) 0.0432(6) Uani 1 1 d .
H14A H 0.1911 0.4235 0.2040 0.052 Uiso 1 1 calc R
C15 C 0.20873(14) 0.33119(13) 0.22993(10) 0.0398(6) Uani 1 1 d .
H15A H 0.1970 0.3399 0.2665 0.048 Uiso 1 1 calc R
C16 C 0.23014(13) 0.26852(11) 0.21439(8) 0.0307(5) Uani 1 1 d .
C121 C 0.25371(17) 0.29244(13) 0.06350(9) 0.0454(6) Uani 1 1 d .
H12A H 0.2401 0.3309 0.0422 0.068 Uiso 1 1 calc R
H12B H 0.2208 0.2557 0.0522 0.068 Uiso 1 1 calc R
H12C H 0.3095 0.2816 0.0580 0.068 Uiso 1 1 calc R
C161 C 0.23735(16) 0.21508(12) 0.25538(9) 0.0425(6) Uani 1 1 d .
H16A H 0.2257 0.2325 0.2911 0.064 Uiso 1 1 calc R
H16B H 0.2912 0.1977 0.2549 0.064 Uiso 1 1 calc R
H16C H 0.1999 0.1803 0.2468 0.064 Uiso 1 1 calc R
C21 C 0.3750 0.3089(2) 0.3750 0.0671(13) Uani 1 2 d S
H21A H 0.3750 0.2627 0.3750 0.080 Uiso 1 2 calc SR
C22 C 0.37497(18) 0.34182(18) 0.32768(14) 0.0682(9) Uani 1 1 d .
H22A H 0.3749 0.3187 0.2947 0.082 Uiso 1 1 calc R
H1 H 0.1250 0.1250 0.0740(13) 0.036(9) Uiso 1 2 d S
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
N1 Zn1 N1 98.43(10) . 8_544
N1 Zn1 Zn1 130.78(5) . 14_445
N1 Zn1 Zn1 130.78(5) 8_544 14_445
C1 N1 C11 117.35(17) . .
C1 N1 Zn1 121.31(14) . .
C11 N1 Zn1 121.33(13) . .
N1 C1 C2 124.3(2) . .
N1 C1 C3 119.04(19) . .
C2 C1 C3 116.6(2) . .
C1 C2 C1 130.1(3) . 8_544
C16 C11 C12 120.7(2) . .
C16 C11 N1 120.05(18) . .
C12 C11 N1 119.21(18) . .
C13 C12 C11 118.6(2) . .
C13 C12 C121 121.1(2) . .
C11 C12 C121 120.3(2) . .
C14 C13 C12 121.1(2) . .
C13 C14 C15 120.1(2) . .
C14 C15 C16 120.7(2) . .
C15 C16 C11 118.7(2) . .
C15 C16 C161 120.5(2) . .
C11 C16 C161 120.8(2) . .
C22 C21 C22 120.2(4) . 3
C21 C22 C22 119.9(2) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 1.9672(17) .
Zn1 N1 1.9673(17) 8_544
Zn1 Zn1 2.4513(9) 14_445
N1 C1 1.334(3) .
N1 C11 1.432(3) .
C1 C2 1.401(2) .
C1 C3 1.509(3) .
C2 C1 1.401(2) 8_544
C11 C16 1.399(3) .
C11 C12 1.402(3) .
C12 C13 1.387(3) .
C12 C121 1.507(3) .
C13 C14 1.377(4) .
C14 C15 1.380(4) .
C15 C16 1.394(3) .
C16 C161 1.506(3) .
C21 C22 1.360(4) .
C21 C22 1.360(4) 3
C22 C22 1.365(8) 2
