#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/82/7008280.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_7008280
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         ' C36 H38 Cl4 N6 Zr2 '
_chemical_formula_sum            'C36 H38 Cl4 N6 Zr2'
_chemical_formula_weight         878.99
_chemical_name_common            (Zr2(mu-N-2,6-C6H3Me2)2Cl4(NC5H5)4)
_chemical_name_systematic
;
[Zr2(mu-N-2,6-C6H3Me2)2Cl4(NC5H5)4]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.0415(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   12.2186(1)
_cell_length_b                   12.4098(2)
_cell_length_c                   12.2628(2)
_cell_measurement_reflns_used    4005
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1795.71(4)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
SIR97 (Altomare et al, 1999)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.01
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7336
_diffrn_reflns_theta_full        27.489
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         2.097
_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    0.914
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             888.000
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.63
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       122.1(157)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.8226
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.010523
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

1.28 0.298 0.962 0.587E-01 0.191
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0276
_refine_ls_wR_factor_gt          0.0253
_refine_ls_wR_factor_ref         0.0253
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                3714
_reflns_number_total             4100
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b500507h.txt
_cod_data_source_block           COMPOUND_15
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
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        1795.70(4)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C36 H38 Cl4 N6 Zr2 '
_cod_database_code               7008280
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_attached_hydrogens
Zr1 Zr -0.11769(1) -0.01429(1) 0.02817(1) 0.0123 1.0000 Uani .
N1 N -0.00480(9) -0.10614(9) -0.02493(9) 0.0140 1.0000 Uani .
N2 N -0.2186(1) -0.1896(1) 0.0284(1) 0.0174 1.0000 Uani .
N3 N -0.2796(1) 0.0787(1) 0.0749(1) 0.0196 1.0000 Uani .
Cl1 Cl -0.07376(3) -0.04338(3) 0.23482(3) 0.0201 1.0000 Uani .
Cl2 Cl -0.25518(3) 0.01367(3) -0.15776(3) 0.0198 1.0000 Uani .
C1 C 0.0172(1) -0.2121(1) -0.05703(11) 0.0146 1.0000 Uani .
C2 C 0.06556(11) -0.28842(11) 0.02811(12) 0.0175 1.0000 Uani .
C3 C 0.09488(13) -0.39030(12) -0.00254(14) 0.0255 1.0000 Uani .
C4 C 0.07642(15) -0.41884(13) -0.11552(16) 0.0336 1.0000 Uani .
C5 C 0.02331(14) -0.34674(13) -0.19802(14) 0.0281 1.0000 Uani .
C6 C -0.00925(11) -0.24422(11) -0.17178(12) 0.0181 1.0000 Uani .
C7 C 0.08413(13) -0.26159(12) 0.15080(12) 0.0225 1.0000 Uani .
C8 C -0.07840(12) -0.17661(12) -0.26707(12) 0.0215 1.0000 Uani .
C9 C -0.23599(11) -0.25015(12) -0.06600(12) 0.0190 1.0000 Uani .
C10 C -0.28081(13) -0.35354(12) -0.07419(13) 0.0242 1.0000 Uani .
C11 C -0.31173(14) -0.39610(13) 0.01746(15) 0.0288 1.0000 Uani .
C12 C -0.29581(14) -0.33484(13) 0.11496(14) 0.0269 1.0000 Uani .
C13 C -0.24799(12) -0.23346(12) 0.11738(12) 0.0214 1.0000 Uani .
C14 C -0.36057(14) 0.02998(13) 0.11158(16) 0.0299 1.0000 Uani .
C15 C -0.45402(14) 0.08395(14) 0.12947(16) 0.0322 1.0000 Uani .
C16 C -0.46349(13) 0.19349(13) 0.11017(13) 0.0248 1.0000 Uani .
C17 C -0.38048(14) 0.24481(13) 0.07249(14) 0.0277 1.0000 Uani .
C18 C -0.29111(13) 0.18511(13) 0.05529(14) 0.0266 1.0000 Uani .
H31 H 0.12946 -0.44371 0.05760 0.0317 1.0000 Uiso .
H41 H 0.10167 -0.49073 -0.13669(16) 0.0407 1.0000 Uiso .
H51 H 0.00734 -0.36869 -0.27909 0.0350 1.0000 Uiso .
H71 H 0.11870 -0.32494 0.19760 0.0270 1.0000 Uiso .
H72 H 0.00987 -0.24369 0.16647 0.0270 1.0000 Uiso .
H73 H 0.13622 -0.19829 0.17014 0.0270 1.0000 Uiso .
H81 H -0.09576 -0.10560 -0.23680 0.0260 1.0000 Uiso .
H82 H -0.15081 -0.21484 -0.30309 0.0260 1.0000 Uiso .
H83 H -0.03462 -0.16457 -0.32449 0.0260 1.0000 Uiso .
H91 H -0.21592 -0.21881 -0.13342 0.0240 1.0000 Uiso .
H101 H -0.29015 -0.39651 -0.14500 0.0297 1.0000 Uiso .
H111 H -0.34562 -0.46982 0.01332 0.0344 1.0000 Uiso .
H121 H -0.31810 -0.36365 0.18227 0.0337 1.0000 Uiso .
H131 H -0.23499 -0.19025 0.18844 0.0270 1.0000 Uiso .
H141 H -0.35401 -0.04942 0.12575(16) 0.0381 1.0000 Uiso .
H151 H -0.51355 0.04420 0.15591(16) 0.0423 1.0000 Uiso .
H161 H -0.52892 0.23481 0.12389 0.0309 1.0000 Uiso .
H171 H -0.38501 0.32414 0.05769 0.0358 1.0000 Uiso .
H181 H -0.23194 0.22300 0.02657 0.0346 1.0000 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   ' 0.0033 0.0016 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 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'N   ' 0.0061 0.0033 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
'Cl  ' 0.1484 0.1585 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  ' -2.9673 0.5597 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_555 Zr1 . N1 . 41.80(3) yes
Zr1 2_555 Zr1 . N1 2_555 39.44(3) yes
N1 . Zr1 . N1 2_555 81.24(5) yes
Zr1 2_555 Zr1 . N2 . 125.24(3) yes
N1 . Zr1 . N2 . 83.55(4) yes
N1 2_555 Zr1 . N2 . 164.28(4) yes
Zr1 2_555 Zr1 . N3 . 145.76(3) yes
N1 . Zr1 . N3 . 170.78(4) yes
N1 2_555 Zr1 . N3 . 106.56(4) yes
N2 . Zr1 . N3 . 88.94(4) yes
Zr1 2_555 Zr1 . Cl1 . 105.86(1) yes
N1 . Zr1 . Cl1 . 105.21(3) yes
N1 2_555 Zr1 . Cl1 . 98.92(3) yes
N2 . Zr1 . Cl1 . 81.25(3) yes
N3 . Zr1 . Cl1 . 78.80(3) yes
Zr1 2_555 Zr1 . Cl2 . 102.82(1) yes
N1 . Zr1 . Cl2 . 97.97(3) yes
N1 2_555 Zr1 . Cl2 . 101.36(3) yes
N2 . Zr1 . Cl2 . 84.63(3) yes
N3 . Zr1 . Cl2 . 75.93(3) yes
Cl1 . Zr1 . Cl2 . 151.177(12) yes
Zr1 . N1 . Zr1 2_555 98.76(5) yes
Zr1 . N1 . C1 . 143.70(9) yes
Zr1 2_555 N1 . C1 . 117.54(8) yes
Zr1 . N2 . C9 . 116.82(9) yes
Zr1 . N2 . C13 . 126.0(1) yes
C9 . N2 . C13 . 116.94(12) yes
Zr1 . N3 . C14 . 124.9(1) yes
Zr1 . N3 . C18 . 117.9(1) yes
C14 . N3 . C18 . 116.99(13) yes
N1 . C1 . C2 . 119.14(11) yes
N1 . C1 . C6 . 121.70(12) yes
C2 . C1 . C6 . 119.16(12) yes
C1 . C2 . C3 . 119.62(13) yes
C1 . C2 . C7 . 121.04(12) yes
C3 . C2 . C7 . 119.34(13) yes
C2 . C3 . C4 . 120.91(14) yes
C3 . C4 . C5 . 119.28(14) yes
C4 . C5 . C6 . 122.01(15) yes
C1 . C6 . C5 . 118.69(13) yes
C1 . C6 . C8 . 123.45(12) yes
C5 . C6 . C8 . 117.71(13) yes
N2 . C9 . C10 . 123.22(14) yes
C9 . C10 . C11 . 118.74(14) yes
C10 . C11 . C12 . 119.03(14) yes
C11 . C12 . C13 . 118.72(14) yes
N2 . C13 . C12 . 123.31(14) yes
N3 . C14 . C15 . 123.15(15) yes
C14 . C15 . C16 . 118.93(15) yes
C15 . C16 . C17 . 118.53(14) yes
C16 . C17 . C18 . 118.99(15) yes
N3 . C18 . C17 . 123.41(14) 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 . Zr1 2_555 3.1474(2) yes
Zr1 . N1 . 2.0229(11) yes
Zr1 . N1 2_555 2.1227(11) yes
Zr1 . N2 . 2.5004(12) yes
Zr1 . N3 . 2.4822(12) yes
Zr1 . Cl1 . 2.4768(3) yes
Zr1 . Cl2 . 2.4805(3) yes
N1 . C1 . 1.4184(16) yes
N2 . C9 . 1.3502(18) yes
N2 . C13 . 1.3489(18) yes
N3 . C14 . 1.333(2) yes
N3 . C18 . 1.343(2) yes
C1 . C2 . 1.4195(19) yes
C1 . C6 . 1.4167(19) yes
C2 . C3 . 1.392(2) yes
C2 . C7 . 1.500(2) yes
C3 . C4 . 1.391(2) yes
C4 . C5 . 1.380(2) yes
C5 . C6 . 1.395(2) yes
C6 . C8 . 1.507(2) yes
C9 . C10 . 1.388(2) yes
C10 . C11 . 1.380(2) yes
C11 . C12 . 1.387(2) yes
C12 . C13 . 1.384(2) yes
C14 . C15 . 1.389(2) yes
C15 . C16 . 1.379(2) yes
C16 . C17 . 1.375(2) yes
C17 . C18 . 1.380(2) yes
