#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:26:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322516.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_4322516
loop_
_publ_author_name
Wood
'Glenn P. A. Yap'
'Darrin S. Richeson'
_publ_section_title
;
 N-Substituted Guanidinate Anions as Ancillary Ligands in Group 4
 Chemistry. Syntheses and Characterization of M{RNC[N(SiMe3)2]NR}2Cl2,
 [M{CyNC[N(SiMe3)2]NCy}Cl3]- (M = Zr, Hf; R =iPr, Cy), and
 Zr{CyNC[N(SiMe3)2]NCy}(CH2Ph)3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5788
_journal_page_last               5794
_journal_paper_doi               10.1021/ic990668i
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C26 H64 Cl2 N6 Si4 Zr'
_chemical_formula_weight         735.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            4
_cell_length_a                   12.5453(17)
_cell_length_b                   17.701(2)
_cell_length_c                   18.012(2)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     3999.8(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.1522
_diffrn_reflns_av_sigmaI/netI    0.1131
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31428
_diffrn_reflns_theta_full        28.77
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.862132
_exptl_absorpt_correction_T_min  0.636696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.851
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1532
_refine_ls_R_factor_gt           0.0654
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1978
_reflns_number_gt                2515
_reflns_number_total             4951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990668i_2.cif
_cod_data_source_block           dr082
_cod_original_cell_volume        3999.9(9)
_cod_database_code               4322516
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
Zr Zr 0.0000 0.17834(4) 0.7500 0.0253(2) Uani 1 2 d S . .
Cl Cl 0.03944(19) 0.27483(13) 0.84117(13) 0.0901(7) Uani 1 1 d . . .
Si1 Si 0.31917(12) 0.00988(9) 0.64906(9) 0.0349(4) Uani 1 1 d . . .
Si2 Si 0.27737(12) 0.14781(9) 0.54767(8) 0.0354(4) Uani 1 1 d . . .
N1 N 0.0614(3) 0.0962(2) 0.6674(2) 0.0274(10) Uani 1 1 d . . .
N2 N 0.1774(3) 0.1615(2) 0.7341(2) 0.0291(10) Uani 1 1 d . . .
N3 N 0.2462(3) 0.0924(2) 0.6269(2) 0.0279(9) Uani 1 1 d . . .
C1 C 0.0237(4) 0.0459(3) 0.6087(3) 0.0320(13) Uani 1 1 d . . .
H1A H 0.0795 0.0417 0.5700 0.038 Uiso 1 1 calc R . .
C2 C -0.0755(4) 0.0784(4) 0.5743(3) 0.0481(16) Uani 1 1 d . . .
H2A H -0.0601 0.1283 0.5548 0.072 Uiso 1 1 calc R . .
H2B H -0.1310 0.0820 0.6116 0.072 Uiso 1 1 calc R . .
H2C H -0.0993 0.0459 0.5343 0.072 Uiso 1 1 calc R . .
C3 C 0.0011(5) -0.0326(3) 0.6399(4) 0.0509(16) Uani 1 1 d . . .
H3A H 0.0657 -0.0531 0.6615 0.076 Uiso 1 1 calc R . .
H3B H -0.0233 -0.0655 0.6004 0.076 Uiso 1 1 calc R . .
H3C H -0.0536 -0.0291 0.6779 0.076 Uiso 1 1 calc R . .
C4 C 0.2826(4) 0.1937(3) 0.7536(3) 0.0366(13) Uani 1 1 d . . .
H4A H 0.3382 0.1665 0.7252 0.044 Uiso 1 1 calc R . .
C5 C 0.3054(5) 0.1844(3) 0.8345(3) 0.0486(16) Uani 1 1 d . . .
H5A H 0.3030 0.1312 0.8473 0.073 Uiso 1 1 calc R . .
H5B H 0.2523 0.2115 0.8632 0.073 Uiso 1 1 calc R . .
H5C H 0.3756 0.2044 0.8456 0.073 Uiso 1 1 calc R . .
C6 C 0.2877(5) 0.2777(3) 0.7328(4) 0.0569(19) Uani 1 1 d . . .
H6A H 0.2717 0.2836 0.6804 0.085 Uiso 1 1 calc R . .
H6B H 0.3586 0.2970 0.7429 0.085 Uiso 1 1 calc R . .
H6C H 0.2359 0.3056 0.7619 0.085 Uiso 1 1 calc R . .
C7 C 0.1644(4) 0.1159(3) 0.6752(3) 0.0255(11) Uani 1 1 d . . .
C8 C 0.2850(4) -0.0191(3) 0.7449(3) 0.0420(14) Uani 1 1 d . . .
H8A H 0.3025 0.0215 0.7790 0.063 Uiso 1 1 calc R . .
H8B H 0.3253 -0.0639 0.7580 0.063 Uiso 1 1 calc R . .
H8C H 0.2094 -0.0300 0.7478 0.063 Uiso 1 1 calc R . .
C9 C 0.2899(5) -0.0708(3) 0.5854(4) 0.0539(17) Uani 1 1 d . . .
H9A H 0.3034 -0.0556 0.5345 0.081 Uiso 1 1 calc R . .
H9B H 0.2158 -0.0855 0.5906 0.081 Uiso 1 1 calc R . .
H9C H 0.3353 -0.1133 0.5980 0.081 Uiso 1 1 calc R . .
C10 C 0.4650(5) 0.0292(4) 0.6415(4) 0.0570(19) Uani 1 1 d . . .
H10A H 0.4844 0.0692 0.6758 0.085 Uiso 1 1 calc R . .
H10B H 0.4818 0.0448 0.5912 0.085 Uiso 1 1 calc R . .
H10C H 0.5046 -0.0162 0.6536 0.085 Uiso 1 1 calc R . .
C11 C 0.3021(5) 0.0856(4) 0.4662(3) 0.0526(16) Uani 1 1 d . . .
H11A H 0.2410 0.0529 0.4585 0.079 Uiso 1 1 calc R . .
H11B H 0.3649 0.0550 0.4752 0.079 Uiso 1 1 calc R . .
H11C H 0.3131 0.1164 0.4223 0.079 Uiso 1 1 calc R . .
C12 C 0.3979(5) 0.2073(4) 0.5609(4) 0.0583(18) Uani 1 1 d . . .
H12A H 0.3890 0.2386 0.6047 0.088 Uiso 1 1 calc R . .
H12B H 0.4080 0.2392 0.5177 0.088 Uiso 1 1 calc R . .
H12C H 0.4598 0.1751 0.5672 0.088 Uiso 1 1 calc R . .
C13 C 0.1630(5) 0.2107(4) 0.5272(3) 0.0525(17) Uani 1 1 d . . .
H13A H 0.0989 0.1807 0.5216 0.079 Uiso 1 1 calc R . .
H13B H 0.1767 0.2383 0.4817 0.079 Uiso 1 1 calc R . .
H13C H 0.1536 0.2462 0.5678 0.079 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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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
N1 Zr N1 98.1(2) 3_556 . ?
N1 Zr N2 59.15(14) 3_556 3_556 ?
N1 Zr N2 109.91(15) . 3_556 ?
N1 Zr N2 109.91(14) 3_556 . ?
N1 Zr N2 59.15(14) . . ?
N2 Zr N2 164.9(2) 3_556 . ?
N1 Zr Cl 94.49(12) 3_556 . ?
N1 Zr Cl 147.82(12) . . ?
N2 Zr Cl 101.99(12) 3_556 . ?
N2 Zr Cl 88.73(11) . . ?
N1 Zr Cl 147.82(12) 3_556 3_556 ?
N1 Zr Cl 94.49(12) . 3_556 ?
N2 Zr Cl 88.73(11) 3_556 3_556 ?
N2 Zr Cl 101.99(12) . 3_556 ?
Cl Zr Cl 90.23(12) . 3_556 ?
N1 Zr C7 29.72(14) 3_556 3_556 ?
N1 Zr C7 109.37(15) . 3_556 ?
N2 Zr C7 29.77(13) 3_556 3_556 ?
N2 Zr C7 139.49(15) . 3_556 ?
Cl Zr C7 96.13(11) . 3_556 ?
Cl Zr C7 118.13(12) 3_556 3_556 ?
N1 Zr C7 109.37(14) 3_556 . ?
N1 Zr C7 29.72(14) . . ?
N2 Zr C7 139.49(15) 3_556 . ?
N2 Zr C7 29.77(13) . . ?
Cl Zr C7 118.13(12) . . ?
Cl Zr C7 96.13(11) 3_556 . ?
C7 Zr C7 131.6(2) 3_556 . ?
N3 Si1 C8 108.6(2) . . ?
N3 Si1 C10 109.8(3) . . ?
C8 Si1 C10 110.2(3) . . ?
N3 Si1 C9 113.0(2) . . ?
C8 Si1 C9 108.4(3) . . ?
C10 Si1 C9 106.8(3) . . ?
N3 Si2 C13 108.7(2) . . ?
N3 Si2 C12 112.9(3) . . ?
C13 Si2 C12 108.4(3) . . ?
N3 Si2 C11 110.1(2) . . ?
C13 Si2 C11 109.1(3) . . ?
C12 Si2 C11 107.5(3) . . ?
C7 N1 C1 123.0(4) . . ?
C7 N1 Zr 95.4(3) . . ?
C1 N1 Zr 140.5(3) . . ?
C7 N2 C4 121.9(4) . . ?
C7 N2 Zr 93.4(3) . . ?
C4 N2 Zr 142.7(3) . . ?
C7 N3 Si1 118.8(3) . . ?
C7 N3 Si2 119.6(3) . . ?
Si1 N3 Si2 121.6(2) . . ?
N1 C1 C2 109.4(4) . . ?
N1 C1 C3 110.4(4) . . ?
C2 C1 C3 110.3(5) . . ?
N2 C4 C5 111.1(4) . . ?
N2 C4 C6 110.6(4) . . ?
C5 C4 C6 109.8(5) . . ?
N2 C7 N1 110.8(4) . . ?
N2 C7 N3 125.2(4) . . ?
N1 C7 N3 124.0(4) . . ?
N2 C7 Zr 56.8(3) . . ?
N1 C7 Zr 54.9(2) . . ?
N3 C7 Zr 170.3(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
Zr N1 2.219(4) 3_556 ?
Zr N1 2.219(4) . ?
Zr N2 2.264(4) 3_556 ?
Zr N2 2.264(4) . ?
Zr Cl 2.420(2) . ?
Zr Cl 2.420(2) 3_556 ?
Zr C7 2.700(5) 3_556 ?
Zr C7 2.700(5) . ?
Si1 N3 1.770(4) . ?
Si1 C8 1.850(6) . ?
Si1 C10 1.866(6) . ?
Si1 C9 1.869(6) . ?
Si2 N3 1.775(4) . ?
Si2 C13 1.853(6) . ?
Si2 C12 1.858(6) . ?
Si2 C11 1.861(6) . ?
N1 C7 1.345(6) . ?
N1 C1 1.462(6) . ?
N2 C7 1.343(6) . ?
N2 C4 1.480(6) . ?
N3 C7 1.408(6) . ?
C1 C2 1.504(7) . ?
C1 C3 1.526(8) . ?
C4 C5 1.494(7) . ?
C4 C6 1.534(8) . ?
