#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/82/7008276.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_7008276
loop_
_publ_author_name
'Dubberley, Stuart R.'
'Evans, Simon'
'Boyd, Catherine L.'
'Mountford, Philip'
_publ_section_title
;
 New and versatile routes to zirconium imido dichloride compounds.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1448
_journal_page_last               1458
_journal_paper_doi               10.1039/b500507h
_journal_year                    2005
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C32 H50 Cl4 N2 O4 Zr2 '
_chemical_formula_sum            'C32 H50 Cl4 N2 O4 Zr2'
_chemical_formula_weight         851.00
_chemical_name_common            (Zr2(mu-N-2,6-C6H3Me2)2Cl4(THF)4)
_chemical_name_systematic
;
[Zr2(mu-N-2,6-C6H3Me2)2Cl4(THF)4]
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7820(3)
_cell_length_b                   17.5806(5)
_cell_length_c                   15.9014(4)
_cell_measurement_reflns_used    2140
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     3573.29(16)
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4063
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.92
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.58
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1722.41
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.46
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       49.4(80)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0221
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1829
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.009
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979,
0.459    0.353E-010.202
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0258
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                1829
_reflns_number_total             2138
_reflns_threshold_expression     >3.00σ(I)
_cod_data_source_file            b500507h.txt
_cod_data_source_block           COMPOUND_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic ' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3573.3(2)
_cod_original_sg_symbol_H-M      'C m c a '
_cod_original_formula_sum        ' C32 H50 Cl4 N2 O4 Zr2 '
_cod_database_code               7008276
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,z
x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
x+1/2,-y,z+1/2
-x+1/2,y,-z+1/2
-x,-y+1/2,z+1/2
x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
Zr1 0.0000 0.064707(13) 0.431031(15) 0.0154 1.0000 Uani
Cl1 -0.18644(3) 0.09114(3) 0.40450(3) 0.0248 1.0000 Uani
N1 0.0000 0.05215(12) 0.56123(13) 0.0165 1.0000 Uani
O1 0.0000 0.1996(1) 0.44766(12) 0.0223 1.0000 Uani
O2 0.0000 0.05457(11) 0.28149(12) 0.0232 1.0000 Uani
C1 0.0000 0.11201(14) 0.62145(15) 0.0171 1.0000 Uani
C2 0.09535(14) 0.1423(1) 0.65176(11) 0.0207 1.0000 Uani
C3 0.09300(16) 0.20419(11) 0.70705(12) 0.0261 1.0000 Uani
C4 -0.000000(7) 0.23598(17) 0.73442(19) 0.0300 1.0000 Uani
C5 0.19998(15) 0.11092(12) 0.62622(13) 0.0273 1.0000 Uani
C6 0.09307(16) 0.24769(11) 0.46006(16) 0.0327 1.0000 Uani
C7 0.0534(4) 0.3287(3) 0.4628(4) 0.0350 0.5000 Uani
C71 0.0491(4) 0.3173(3) 0.5087(4) 0.0325 0.5000 Uani
C8 -0.09222(16) 0.04417(18) 0.22793(14) 0.0428 1.0000 Uani
C9 -0.0541(7) 0.0226(5) 0.1418(6) 0.0392 0.5000 Uani
C91 -0.0564(8) -0.0058(5) 0.1585(5) 0.0360 0.5000 Uani
H31 0.16063 0.22616 0.72727 0.0321 1.0000 Uiso
H41 -0.000000 0.28078 0.77317 0.0343 1.0000 Uiso
H51 0.25662 0.14048 0.65475 0.0324 1.0000 Uiso
H52 0.20481 0.05623 0.64306 0.0324 1.0000 Uiso
H53 0.20821 0.11532 0.56387 0.0324 1.0000 Uiso
H61 0.12849 0.23374 0.51397 0.0431 1.0000 Uiso
H62 0.14317 0.24123 0.41229 0.0431 1.0000 Uiso
H71 0.1014 0.3621 0.4961 0.0470 0.5000 Uiso
H72 0.0434 0.3507 0.4054 0.0470 0.5000 Uiso
H711 0.0386 0.3053 0.5696 0.0433 0.5000 Uiso
H712 0.0959 0.3626 0.5032 0.0433 0.5000 Uiso
H81 -0.13773 0.00359 0.25250 0.0578 1.0000 Uiso
H82 -0.13235 0.09292 0.22468 0.0578 1.0000 Uiso
H91 -0.0960 -0.0209 0.1194 0.0622 0.5000 Uiso
H92 -0.0568 0.0660 0.1012 0.0622 0.5000 Uiso
H911 -0.0583 -0.0605 0.1755 0.0478 0.5000 Uiso
H912 -0.1018 0.0020 0.1081 0.0478 0.5000 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C   ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H   ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'N   ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O   ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Cl  ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'Zr  ' -2.9650 0.5600 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572
87.6627 2.0693 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Zr1 2_556 Zr1 . Cl1 . 104.748(12) yes
Zr1 2_556 Zr1 . Cl1 5_555 104.748(12) yes
Cl1 . Zr1 . Cl1 5_555 150.49(2) yes
Zr1 2_556 Zr1 . N1 . 39.96(6) yes
Cl1 . Zr1 . N1 . 100.965(16) yes
Cl1 5_555 Zr1 . N1 . 100.965(16) yes
Zr1 2_556 Zr1 . N1 2_556 40.53(6) yes
Cl1 . Zr1 . N1 2_556 101.447(16) yes
Cl1 5_555 Zr1 . N1 2_556 101.447(16) yes
N1 . Zr1 . N1 2_556 80.49(9) yes
Zr1 2_556 Zr1 . O1 . 129.69(5) yes
Cl1 . Zr1 . O1 . 80.303(15) yes
Cl1 5_555 Zr1 . O1 . 80.303(15) yes
N1 . Zr1 . O1 . 89.72(7) yes
N1 2_556 Zr1 . O1 . 170.21(7) yes
Zr1 2_556 Zr1 . O2 . 129.67(5) yes
Cl1 . Zr1 . O2 . 80.989(15) yes
Cl1 5_555 Zr1 . O2 . 80.989(15) yes
N1 . Zr1 . O2 . 169.63(7) yes
N1 2_556 Zr1 . O2 . 89.14(8) yes
O1 . Zr1 . O2 . 100.65(7) yes
Zr1 . N1 . Zr1 2_556 99.51(9) yes
Zr1 . N1 . C1 . 126.21(16) yes
Zr1 2_556 N1 . C1 . 134.27(17) yes
Zr1 . O1 . C6 . 125.8(1) yes
Zr1 . O1 . C6 5_555 125.8(1) yes
C6 . O1 . C6 5_555 107.8(2) yes
Zr1 . O2 . C8 . 126.1(1) yes
Zr1 . O2 . C8 5_555 126.1(1) yes
C8 . O2 . C8 5_555 107.1(2) yes
N1 . C1 . C2 . 120.51(11) yes
N1 . C1 . C2 5_555 120.51(11) yes
C2 . C1 . C2 5_555 119.0(2) yes
C1 . C2 . C3 . 119.22(18) yes
C1 . C2 . C5 . 122.46(16) yes
C3 . C2 . C5 . 118.32(16) yes
C2 . C3 . C4 . 122.01(19) yes
C3 . C4 . C3 5_555 118.4(3) yes
O1 . C6 . C7 . 105.9(2) yes
O1 . C6 . C71 . 103.1(2) yes
C6 . C7 . C71 5_555 100.3(3) yes
C6 . C71 . C7 5_555 100.3(4) yes
O2 . C8 . C9 . 107.4(4) yes
O2 . C8 . C91 . 104.9(4) yes
C8 . C9 . C91 5_555 103.0(8) yes
C8 . C91 . C9 5_555 102.9(8) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 . Cl1 . 2.4643(4) yes
Zr1 . Cl1 5_555 2.4643(4) yes
Zr1 . N1 . 2.082(2) yes
Zr1 . N1 2_556 2.058(2) yes
Zr1 . O1 . 2.3869(18) yes
Zr1 . O2 . 2.3845(19) yes
N1 . C1 . 1.423(3) yes
O1 . C6 . 1.472(2) yes
O1 . C6 5_555 1.472(2) yes
O2 . C8 . 1.466(2) yes
O2 . C8 5_555 1.466(2) yes
C1 . C2 . 1.415(2) yes
C1 . C2 5_555 1.415(2) yes
C2 . C3 . 1.399(3) yes
C2 . C5 . 1.503(3) yes
C3 . C4 . 1.384(2) yes
C6 . C7 . 1.512(5) yes
C6 . C71 . 1.553(5) yes
C7 . C71 5_555 1.513(6) yes
C8 . C9 . 1.50(1) yes
C8 . C91 . 1.48(1) yes
C9 . C91 5_555 1.521(6) yes
