#------------------------------------------------------------------------------
#$Date: 2025-08-22 00:24:23 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301857 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/51/7115187.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_7115187
loop_
_publ_author_name
'Daniele, Stephane'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
_publ_section_title
;
 meta- and para-Bis[zirconyl(IV)amino]cyclophanes; 1,3- or
 1,4-C6H4[N(SiMe3)]2 as bridging ligands†
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1909
_journal_paper_doi               10.1039/a903921j
_journal_year                    1999
_chemical_formula_structural     '[{Zr(NMe2)2(m-Me3SiNC6H4NSiMe3)}2]'
_chemical_formula_sum            'C32 H68 N8 Si4 Zr2'
_chemical_formula_weight         859.74
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.55(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.234(2)
_cell_length_b                   17.771(4)
_cell_length_c                   18.860(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     4495.7(16)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       ω--2θ
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4123
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_obs          0.0306
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0243P)²+3.0789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0774
_refine_ls_wR_factor_obs         0.0718
_reflns_number_observed          3288
_reflns_number_total             3963
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903921j.txt
_cod_data_source_block           DHL-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+3.0789P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+3.0789P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4495.6(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7115187
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Zr Zr 0.19643(2) -0.096068(15) 0.185268(14) 0.02089(9) Uani 1 d .
Si1 Si 0.33930(5) -0.04669(4) 0.36003(4) 0.0243(2) Uani 1 d .
Si2 Si 0.00257(6) -0.20490(4) 0.43317(4) 0.0240(2) Uani 1 d .
N1 N 0.2211(2) -0.05047(12) 0.29217(12) 0.0208(5) Uani 1 d .
N2 N -0.0512(2) -0.12588(13) 0.38133(12) 0.0234(5) Uani 1 d .
N3 N 0.2599(2) -0.02971(14) 0.12663(13) 0.0291(5) Uani 1 d .
N4 N 0.2695(2) -0.19621(13) 0.19708(13) 0.0286(5) Uani 1 d .
C1 C 0.1420(2) -0.03018(15) 0.31918(14) 0.0203(6) Uani 1 d .
C2 C 0.0857(2) -0.08545(14) 0.33757(14) 0.0207(6) Uani 1 d .
H2 H 0.0998(2) -0.13668(14) 0.33076(14) 0.025 Uiso 1 calc R
C3 C 0.0087(2) -0.06889(14) 0.36582(14) 0.0196(5) Uani 1 d .
C4 C -0.0106(2) 0.0066(2) 0.3755(2) 0.0264(6) Uani 1 d .
H4 H -0.0609(2) 0.0198(2) 0.3961(2) 0.032 Uiso 1 calc R
C5 C 0.0435(2) 0.0625(2) 0.3553(2) 0.0315(7) Uani 1 d .
H5 H 0.0285(2) 0.1138(2) 0.3610(2) 0.038 Uiso 1 calc R
C6 C 0.1190(2) 0.0453(2) 0.3270(2) 0.0277(6) Uani 1 d .
H6 H 0.1549(2) 0.0844(2) 0.3131(2) 0.033 Uiso 1 calc R
C7 C 0.3756(2) 0.0513(2) 0.3922(2) 0.0409(8) Uani 1 d .
H7A H 0.3742(2) 0.0825(2) 0.3490(2) 0.061 Uiso 1 calc R
H7B H 0.4431(2) 0.0514(2) 0.4292(2) 0.061 Uiso 1 calc R
H7C H 0.3288(2) 0.0715(2) 0.4153(2) 0.061 Uiso 1 calc R
C8 C 0.4332(2) -0.0844(2) 0.3206(2) 0.0433(8) Uani 1 d .
H8A H 0.4324(2) -0.0544(2) 0.2768(2) 0.065 Uiso 1 calc R
H8B H 0.4171(2) -0.1369(2) 0.3052(2) 0.065 Uiso 1 calc R
H8C H 0.4996(2) -0.0820(2) 0.3589(2) 0.065 Uiso 1 calc R
C9 C 0.3425(2) -0.1047(2) 0.4424(2) 0.0365(7) Uani 1 d .
H9A H 0.3235(2) -0.1565(2) 0.4262(2) 0.055 Uiso 1 calc R
H9B H 0.2957(2) -0.0840(2) 0.4654(2) 0.055 Uiso 1 calc R
H9C H 0.4101(2) -0.1042(2) 0.4793(2) 0.055 Uiso 1 calc R
C10 C -0.0877(2) -0.2473(2) 0.4735(2) 0.0364(7) Uani 1 d .
H10A H -0.1071(2) -0.2097(2) 0.5040(2) 0.055 Uiso 1 calc R
H10B H -0.0566(2) -0.2904(2) 0.5051(2) 0.055 Uiso 1 calc R
H10C H -0.1469(2) -0.2642(2) 0.4326(2) 0.055 Uiso 1 calc R
C11 C 0.1153(2) -0.1748(2) 0.5123(2) 0.0396(8) Uani 1 d .
H11A H 0.1638(2) -0.1523(2) 0.4920(2) 0.059 Uiso 1 calc R
H11B H 0.1453(2) -0.2187(2) 0.5431(2) 0.059 Uiso 1 calc R
H11C H 0.0961(2) -0.1377(2) 0.5434(2) 0.059 Uiso 1 calc R
C12 C 0.0386(2) -0.2772(2) 0.3754(2) 0.0369(7) Uani 1 d .
H12A H 0.0862(2) -0.2554(2) 0.3538(2) 0.055 Uiso 1 calc R
H12B H -0.0209(2) -0.2941(2) 0.3347(2) 0.055 Uiso 1 calc R
H12C H 0.0693(2) -0.3202(2) 0.4072(2) 0.055 Uiso 1 calc R
C13 C 0.3163(2) 0.0396(2) 0.1480(2) 0.0388(8) Uani 1 d .
H13A H 0.3283(2) 0.0499(2) 0.2013(2) 0.058 Uiso 1 calc R
H13B H 0.2783(2) 0.0812(2) 0.1176(2) 0.058 Uiso 1 calc R
H13C H 0.3802(2) 0.0345(2) 0.1394(2) 0.058 Uiso 1 calc R
C14 C 0.2399(3) -0.0475(2) 0.0477(2) 0.0441(8) Uani 1 d .
H14A H 0.2018(3) -0.0945(2) 0.0352(2) 0.066 Uiso 1 calc R
H14B H 0.3032(3) -0.0535(2) 0.0382(2) 0.066 Uiso 1 calc R
H14C H 0.2014(3) -0.0066(2) 0.0164(2) 0.066 Uiso 1 calc R
C15 C 0.3432(2) -0.2227(2) 0.1655(2) 0.0434(8) Uani 1 d .
H15A H 0.3532(2) -0.1846(2) 0.1311(2) 0.065 Uiso 1 calc R
H15B H 0.3200(2) -0.2696(2) 0.1378(2) 0.065 Uiso 1 calc R
H15C H 0.4064(2) -0.2318(2) 0.2061(2) 0.065 Uiso 1 calc R
C16 C 0.2526(3) -0.2511(2) 0.2484(2) 0.0459(8) Uani 1 d .
H16A H 0.2025(3) -0.2318(2) 0.2689(2) 0.069 Uiso 1 calc R
H16B H 0.3151(3) -0.2604(2) 0.2897(2) 0.069 Uiso 1 calc R
H16C H 0.2287(3) -0.2982(2) 0.2214(2) 0.069 Uiso 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'
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
N3 Zr N4 105.29(10) . .
N3 Zr N1 109.83(9) . .
N4 Zr N1 108.56(9) . .
N3 Zr N2 110.54(9) . 6_556
N4 Zr N2 102.14(9) . 6_556
N1 Zr N2 119.32(8) . 6_556
N3 Zr C3 108.48(9) . 6_556
N4 Zr C3 128.74(8) . 6_556
N1 Zr C3 94.86(8) . 6_556
N2 Zr C3 29.49(8) 6_556 6_556
N1 Si1 C9 110.00(13) . .
N1 Si1 C7 111.78(13) . .
C9 Si1 C7 108.7(2) . .
N1 Si1 C8 109.80(13) . .
C9 Si1 C8 108.4(2) . .
C7 Si1 C8 108.0(2) . .
N2 Si2 C10 108.91(12) . .
N2 Si2 C12 112.58(13) . .
C10 Si2 C12 108.82(14) . .
N2 Si2 C11 108.52(13) . .
C10 Si2 C11 108.43(15) . .
C12 Si2 C11 109.5(2) . .
C1 N1 Si1 114.3(2) . .
C1 N1 Zr 122.9(2) . .
Si1 N1 Zr 122.23(11) . .
C3 N2 Si2 120.9(2) . .
C3 N2 Zr 103.7(2) . 6_556
Si2 N2 Zr 134.60(12) . 6_556
C13 N3 C14 111.7(2) . .
C13 N3 Zr 130.5(2) . .
C14 N3 Zr 117.5(2) . .
C15 N4 C16 111.2(3) . .
C15 N4 Zr 130.8(2) . .
C16 N4 Zr 117.9(2) . .
C2 C1 C6 118.5(2) . .
C2 C1 N1 120.1(2) . .
C6 C1 N1 121.3(2) . .
C1 C2 C3 122.6(2) . .
C4 C3 C2 117.8(2) . .
C4 C3 N2 120.1(2) . .
C2 C3 N2 122.0(2) . .
C4 C3 Zr 89.0(2) . 6_556
C2 C3 Zr 133.9(2) . 6_556
N2 C3 Zr 46.81(12) . 6_556
C5 C4 C3 120.0(3) . .
C6 C5 C4 121.5(3) . .
C5 C6 C1 119.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr N3 2.025(2) .
Zr N4 2.036(2) .
Zr N1 2.091(2) .
Zr N2 2.097(2) 6_556
Zr C3 2.794(3) 6_556
Si1 N1 1.741(2) .
Si1 C9 1.852(3) .
Si1 C7 1.859(3) .
Si1 C8 1.859(3) .
Si2 N2 1.736(2) .
Si2 C10 1.857(3) .
Si2 C12 1.865(3) .
Si2 C11 1.868(3) .
N1 C1 1.429(3) .
N2 C3 1.416(3) .
N2 Zr 2.097(2) 6_556
N3 C13 1.452(4) .
N3 C14 1.455(4) .
N4 C15 1.448(4) .
N4 C16 1.451(4) .
C1 C2 1.383(4) .
C1 C6 1.401(4) .
C2 C3 1.401(4) .
C3 C4 1.394(4) .
C3 Zr 2.794(3) 6_556
C4 C5 1.387(4) .
C5 C6 1.383(4) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 5257300
