#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/82/4318294.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_4318294
loop_
_publ_author_name
'Jean-Sébastien M. Lehn'
'David M. Hoffman'
_publ_section_title
;
 Synthesis and Structures of Zirconium Amide-Iodide Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4063
_journal_page_last               4067
_journal_paper_doi               10.1021/ic025630b
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C12 H36 I2 N6 Zr2'
_chemical_formula_weight         700.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.487(1)
_cell_angle_beta                 99.479(1)
_cell_angle_gamma                117.836(1)
_cell_formula_units_Z            2
_cell_length_a                   8.5884(6)
_cell_length_b                   8.7949(6)
_cell_length_c                   18.1676(12)
_cell_measurement_reflns_used    5189
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.30
_cell_volume                     1185.48(14)
_computing_cell_refinement       'Siemens SAINT software (Siemens, 1996)'
_computing_data_collection       'Siemens SMART software (Siemens, 1996)'
_computing_data_reduction        'Siemens SAINT software (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 1K
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       CCD
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6179
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    3.489
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5563
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Flat plate'
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0353P)²+1.8055P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                3689
_reflns_number_total             4072
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic025630b_s1_1.cif
_cod_data_source_block           k383[Zr(NMe2)3I]2
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_formula_sum        'C12 H36 N6 I2 Zr2'
_cod_database_code               4318294
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.82114(4) 0.54680(4) 0.385654(15) 0.03919(10) Uani 1 1 d . . .
I2 I 0.15930(4) 0.86567(4) 0.112590(17) 0.03992(10) Uani 1 1 d . . .
Zr1 Zr 0.64791(4) 0.75548(4) 0.33709(2) 0.02368(10) Uani 1 1 d . . .
Zr2 Zr 0.35986(5) 0.68371(4) 0.16196(2) 0.02448(10) Uani 1 1 d . . .
N1 N 0.5701(4) 0.6084(4) 0.22316(17) 0.0260(6) Uani 1 1 d . . .
N2 N 0.5052(4) 0.8846(4) 0.26385(17) 0.0262(6) Uani 1 1 d . . .
N3 N 0.8806(4) 0.9781(4) 0.3721(2) 0.0352(7) Uani 1 1 d . . .
N4 N 0.4799(4) 0.6848(4) 0.40898(19) 0.0327(7) Uani 1 1 d . . .
N5 N 0.4444(5) 0.6966(5) 0.0646(2) 0.0378(8) Uani 1 1 d . . .
N6 N 0.1446(4) 0.4578(4) 0.1678(2) 0.0327(7) Uani 1 1 d . . .
C1 C 0.7410(5) 0.6910(6) 0.1956(2) 0.0363(9) Uani 1 1 d . . .
H1A H 0.7939 0.8150 0.2058 0.054 Uiso 1 1 calc R . .
H1B H 0.7166 0.6565 0.1423 0.054 Uiso 1 1 calc R . .
H1C H 0.8229 0.6549 0.2209 0.054 Uiso 1 1 calc R . .
C2 C 0.4974(6) 0.4180(5) 0.2078(3) 0.0396(10) Uani 1 1 d . . .
H2A H 0.3858 0.3599 0.2245 0.059 Uiso 1 1 calc R . .
H2B H 0.5823 0.3868 0.2344 0.059 Uiso 1 1 calc R . .
H2C H 0.4770 0.3839 0.1547 0.059 Uiso 1 1 calc R . .
C3 C 0.4073(6) 0.9432(6) 0.3081(2) 0.0381(9) Uani 1 1 d . . .
H3A H 0.3242 0.8470 0.3290 0.057 Uiso 1 1 calc R . .
H3B H 0.3425 0.9876 0.2758 0.057 Uiso 1 1 calc R . .
H3C H 0.4920 1.0330 0.3482 0.057 Uiso 1 1 calc R . .
C4 C 0.6327(6) 1.0374(5) 0.2331(3) 0.0397(10) Uani 1 1 d . . .
H4A H 0.6992 1.0036 0.2048 0.060 Uiso 1 1 calc R . .
H4B H 0.7145 1.1266 0.2739 0.060 Uiso 1 1 calc R . .
H4C H 0.5666 1.0805 0.2008 0.060 Uiso 1 1 calc R . .
C5 C 1.0512(6) 1.0273(6) 0.3502(3) 0.0521(12) Uani 1 1 d . . .
H5A H 1.0371 0.9380 0.3132 0.078 Uiso 1 1 calc R . .
H5B H 1.1400 1.0422 0.3937 0.078 Uiso 1 1 calc R . .
H5C H 1.0894 1.1344 0.3293 0.078 Uiso 1 1 calc R . .
C6 C 0.8946(7) 1.1122(6) 0.4262(3) 0.0550(13) Uani 1 1 d . . .
H6A H 0.7806 1.0756 0.4401 0.083 Uiso 1 1 calc R . .
H6B H 0.9280 1.2174 0.4041 0.083 Uiso 1 1 calc R . .
H6C H 0.9845 1.1325 0.4701 0.083 Uiso 1 1 calc R . .
C7 C 0.4651(7) 0.7747(6) 0.4746(3) 0.0514(12) Uani 1 1 d . . .
H7A H 0.5561 0.8944 0.4825 0.077 Uiso 1 1 calc R . .
H7B H 0.4813 0.7216 0.5183 0.077 Uiso 1 1 calc R . .
H7C H 0.3483 0.7672 0.4664 0.077 Uiso 1 1 calc R . .
C8 C 0.3429(6) 0.5032(6) 0.3952(3) 0.0495(11) Uani 1 1 d . . .
H8A H 0.3576 0.4457 0.3529 0.074 Uiso 1 1 calc R . .
H8B H 0.2257 0.4950 0.3848 0.074 Uiso 1 1 calc R . .
H8C H 0.3549 0.4490 0.4390 0.074 Uiso 1 1 calc R . .
C9 C 0.5979(8) 0.8268(8) 0.0377(3) 0.0638(15) Uani 1 1 d . . .
H9A H 0.6906 0.9011 0.0801 0.096 Uiso 1 1 calc R . .
H9B H 0.5602 0.8948 0.0072 0.096 Uiso 1 1 calc R . .
H9C H 0.6437 0.7698 0.0083 0.096 Uiso 1 1 calc R . .
C10 C 0.3044(8) 0.5809(8) 0.0012(3) 0.0643(15) Uani 1 1 d . . .
H10A H 0.2036 0.4970 0.0194 0.096 Uiso 1 1 calc R . .
H10B H 0.3504 0.5223 -0.0271 0.096 Uiso 1 1 calc R . .
H10C H 0.2665 0.6470 -0.0306 0.096 Uiso 1 1 calc R . .
C11 C 0.0398(6) 0.4618(6) 0.2221(3) 0.0484(11) Uani 1 1 d . . .
H11A H 0.0949 0.5767 0.2491 0.073 Uiso 1 1 calc R . .
H11B H 0.0354 0.3813 0.2568 0.073 Uiso 1 1 calc R . .
H11C H -0.0802 0.4299 0.1962 0.073 Uiso 1 1 calc R . .
C12 C 0.0608(7) 0.2853(6) 0.1240(3) 0.0536(12) Uani 1 1 d . . .
H12A H 0.1339 0.2844 0.0895 0.080 Uiso 1 1 calc R . .
H12B H -0.0567 0.2572 0.0964 0.080 Uiso 1 1 calc R . .
H12C H 0.0504 0.2010 0.1575 0.080 Uiso 1 1 calc R . .
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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_geom_angle_publ_flag
N4 Zr1 N3 115.58(14) . . ?
N4 Zr1 N1 121.62(13) . . ?
N3 Zr1 N1 122.60(13) . . ?
N4 Zr1 N2 95.11(12) . . ?
N3 Zr1 N2 94.42(12) . . ?
N1 Zr1 N2 76.81(11) . . ?
N4 Zr1 I1 96.25(10) . . ?
N3 Zr1 I1 91.73(10) . . ?
N1 Zr1 I1 86.75(8) . . ?
N2 Zr1 I1 163.25(7) . . ?
N6 Zr2 N5 114.76(15) . . ?
N6 Zr2 N2 119.99(13) . . ?
N5 Zr2 N2 124.83(13) . . ?
N6 Zr2 N1 94.82(12) . . ?
N5 Zr2 N1 93.25(13) . . ?
N2 Zr2 N1 76.42(10) . . ?
N6 Zr2 I2 96.23(9) . . ?
N5 Zr2 I2 91.96(10) . . ?
N2 Zr2 I2 88.63(8) . . ?
N1 Zr2 I2 164.50(7) . . ?
C2 N1 C1 107.0(3) . . ?
C2 N1 Zr1 124.3(3) . . ?
C1 N1 Zr1 102.5(2) . . ?
C2 N1 Zr2 109.6(2) . . ?
C1 N1 Zr2 111.7(2) . . ?
Zr1 N1 Zr2 101.44(11) . . ?
C4 N2 C3 107.7(3) . . ?
C4 N2 Zr2 102.8(2) . . ?
C3 N2 Zr2 121.4(2) . . ?
C4 N2 Zr1 112.8(2) . . ?
C3 N2 Zr1 111.2(2) . . ?
Zr2 N2 Zr1 100.79(11) . . ?
C6 N3 C5 111.2(4) . . ?
C6 N3 Zr1 121.2(3) . . ?
C5 N3 Zr1 127.5(3) . . ?
C8 N4 C7 110.9(3) . . ?
C8 N4 Zr1 114.8(3) . . ?
C7 N4 Zr1 134.3(3) . . ?
C10 N5 C9 110.1(4) . . ?
C10 N5 Zr2 113.7(3) . . ?
C9 N5 Zr2 133.6(3) . . ?
C11 N6 C12 110.7(4) . . ?
C11 N6 Zr2 116.4(3) . . ?
C12 N6 Zr2 132.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Zr1 2.9357(4) . ?
I2 Zr2 2.9193(4) . ?
Zr1 N4 2.007(3) . ?
Zr1 N3 2.012(3) . ?
Zr1 N1 2.216(3) . ?
Zr1 N2 2.336(3) . ?
Zr2 N6 2.007(3) . ?
Zr2 N5 2.008(3) . ?
Zr2 N2 2.237(3) . ?
Zr2 N1 2.336(3) . ?
N1 C2 1.483(5) . ?
N1 C1 1.486(5) . ?
N2 C4 1.486(5) . ?
N2 C3 1.487(5) . ?
N3 C6 1.449(6) . ?
N3 C5 1.451(5) . ?
N4 C8 1.453(6) . ?
N4 C7 1.458(5) . ?
N5 C10 1.451(6) . ?
N5 C9 1.462(6) . ?
N6 C11 1.449(6) . ?
N6 C12 1.463(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Zr1 N1 C2 -51.5(3) . . . . ?
N3 Zr1 N1 C2 133.8(3) . . . . ?
N2 Zr1 N1 C2 -139.4(3) . . . . ?
I1 Zr1 N1 C2 43.8(3) . . . . ?
N4 Zr1 N1 C1 -172.4(2) . . . . ?
N3 Zr1 N1 C1 12.9(3) . . . . ?
N2 Zr1 N1 C1 99.7(2) . . . . ?
I1 Zr1 N1 C1 -77.1(2) . . . . ?
N4 Zr1 N1 Zr2 72.01(16) . . . . ?
N3 Zr1 N1 Zr2 -102.67(15) . . . . ?
N2 Zr1 N1 Zr2 -15.88(11) . . . . ?
I1 Zr1 N1 Zr2 167.35(10) . . . . ?
N6 Zr2 N1 C2 29.9(3) . . . . ?
N5 Zr2 N1 C2 -85.3(3) . . . . ?
N2 Zr2 N1 C2 149.7(3) . . . . ?
I2 Zr2 N1 C2 165.3(2) . . . . ?
N6 Zr2 N1 C1 148.4(2) . . . . ?
N5 Zr2 N1 C1 33.2(3) . . . . ?
N2 Zr2 N1 C1 -91.9(2) . . . . ?
I2 Zr2 N1 C1 -76.2(4) . . . . ?
N6 Zr2 N1 Zr1 -103.09(14) . . . . ?
N5 Zr2 N1 Zr1 141.71(14) . . . . ?
N2 Zr2 N1 Zr1 16.63(11) . . . . ?
I2 Zr2 N1 Zr1 32.3(4) . . . . ?
N6 Zr2 N2 C4 -171.3(2) . . . . ?
N5 Zr2 N2 C4 16.5(3) . . . . ?
N1 Zr2 N2 C4 100.9(2) . . . . ?
I2 Zr2 N2 C4 -74.9(2) . . . . ?
N6 Zr2 N2 C3 -51.2(3) . . . . ?
N5 Zr2 N2 C3 136.7(3) . . . . ?
N1 Zr2 N2 C3 -138.9(3) . . . . ?
I2 Zr2 N2 C3 45.2(3) . . . . ?
N6 Zr2 N2 Zr1 72.02(15) . . . . ?
N5 Zr2 N2 Zr1 -100.15(16) . . . . ?
N1 Zr2 N2 Zr1 -15.72(11) . . . . ?
I2 Zr2 N2 Zr1 168.42(9) . . . . ?
N4 Zr1 N2 C4 146.3(3) . . . . ?
N3 Zr1 N2 C4 30.1(3) . . . . ?
N1 Zr1 N2 C4 -92.4(3) . . . . ?
I1 Zr1 N2 C4 -81.1(4) . . . . ?
N4 Zr1 N2 C3 25.2(3) . . . . ?
N3 Zr1 N2 C3 -91.0(3) . . . . ?
N1 Zr1 N2 C3 146.5(3) . . . . ?
I1 Zr1 N2 C3 157.8(2) . . . . ?
N4 Zr1 N2 Zr2 -104.75(13) . . . . ?
N3 Zr1 N2 Zr2 139.04(13) . . . . ?
N1 Zr1 N2 Zr2 16.56(11) . . . . ?
I1 Zr1 N2 Zr2 27.8(3) . . . . ?
N4 Zr1 N3 C6 -25.5(4) . . . . ?
N1 Zr1 N3 C6 149.5(3) . . . . ?
N2 Zr1 N3 C6 72.3(4) . . . . ?
I1 Zr1 N3 C6 -123.2(4) . . . . ?
N4 Zr1 N3 C5 153.4(4) . . . . ?
N1 Zr1 N3 C5 -31.6(4) . . . . ?
N2 Zr1 N3 C5 -108.8(4) . . . . ?
I1 Zr1 N3 C5 55.7(4) . . . . ?
N3 Zr1 N4 C8 -161.5(3) . . . . ?
N1 Zr1 N4 C8 23.4(4) . . . . ?
N2 Zr1 N4 C8 101.1(3) . . . . ?
I1 Zr1 N4 C8 -66.6(3) . . . . ?
N3 Zr1 N4 C7 16.8(5) . . . . ?
N1 Zr1 N4 C7 -158.2(4) . . . . ?
N2 Zr1 N4 C7 -80.6(4) . . . . ?
I1 Zr1 N4 C7 111.7(4) . . . . ?
N6 Zr2 N5 C10 25.0(4) . . . . ?
N2 Zr2 N5 C10 -162.4(3) . . . . ?
N1 Zr2 N5 C10 121.9(3) . . . . ?
I2 Zr2 N5 C10 -72.7(3) . . . . ?
N6 Zr2 N5 C9 -175.4(4) . . . . ?
N2 Zr2 N5 C9 -2.8(5) . . . . ?
N1 Zr2 N5 C9 -78.5(4) . . . . ?
I2 Zr2 N5 C9 86.9(4) . . . . ?
N5 Zr2 N6 C11 -158.1(3) . . . . ?
N2 Zr2 N6 C11 29.0(4) . . . . ?
N1 Zr2 N6 C11 106.1(3) . . . . ?
I2 Zr2 N6 C11 -63.1(3) . . . . ?
N5 Zr2 N6 C12 17.2(4) . . . . ?
N2 Zr2 N6 C12 -155.8(4) . . . . ?
N1 Zr2 N6 C12 -78.7(4) . . . . ?
I2 Zr2 N6 C12 112.2(4) . . . . ?
