#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:46:53 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178667 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/78/4077802.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_4077802
loop_
_publ_author_name
'Morton, Colin'
'Munslow, Ian J.'
'Sanders, Christopher J.'
'Alcock, Nathaniel W.'
'Scott, Peter'
_publ_section_title
;
 Triamidoamine Chemistry of Zirconium
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4608
_journal_paper_doi               10.1021/om990347e
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C31 H64 N4 Si3 Zr'
_chemical_formula_weight         668.35
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.883(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0082(15)
_cell_length_b                   18.663(3)
_cell_length_c                   18.131(3)
_cell_measurement_reflns_used    8927
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      1.61
_cell_volume                     3844.6(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22792
_diffrn_reflns_theta_full        28.54
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         8927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0452P)²+0.0712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                6868
_reflns_number_total             8927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990347e.cif
_cod_data_source_block
'cicm_compound_1_in_Scott_and_co-workers_Triamidoamine chemistry....'
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3844.7(9)
_cod_original_sg_symbol_H-M      P(2)1/n
_cod_database_code               4077802
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zr1 Zr 0.199150(15) 0.246785(8) 0.611783(10) 0.02439(6) Uani 1 1 d .
Si1 Si -0.00317(5) 0.22163(3) 0.70798(3) 0.03164(12) Uani 1 1 d .
N1 N 0.06043(13) 0.27343(9) 0.65247(9) 0.0310(3) Uani 1 1 d .
C1 C -0.06306(18) 0.31659(11) 0.52512(12) 0.0431(5) Uani 1 1 d .
H1A H -0.1188 0.2761 0.5182 0.052 Uiso 1 1 calc R
H1B H -0.1063 0.3582 0.4956 0.052 Uiso 1 1 calc R
Si2 Si 0.34651(5) 0.40945(3) 0.62632(3) 0.03025(12) Uani 1 1 d .
N2 N 0.26682(13) 0.33738(8) 0.57470(9) 0.0320(3) Uani 1 1 d .
C2 C -0.01117(19) 0.33531(11) 0.61082(12) 0.0404(5) Uani 1 1 d .
H2A H 0.0390 0.3785 0.6173 0.048 Uiso 1 1 calc R
H2B H -0.0750 0.3456 0.6328 0.048 Uiso 1 1 calc R
Si3 Si 0.25023(5) 0.11861(3) 0.49227(3) 0.03443(13) Uani 1 1 d .
N3 N 0.15466(13) 0.16653(8) 0.52831(9) 0.0295(3) Uani 1 1 d .
C3 C 0.08437(19) 0.35955(11) 0.46776(12) 0.0450(5) Uani 1 1 d .
H3A H 0.0680 0.4038 0.4925 0.054 Uiso 1 1 calc R
H3B H 0.0482 0.3643 0.4106 0.054 Uiso 1 1 calc R
N4 N 0.03442(14) 0.29658(9) 0.49603(9) 0.0351(4) Uani 1 1 d .
C4 C 0.21648(19) 0.34860(12) 0.48872(11) 0.0434(5) Uani 1 1 d .
H4A H 0.2328 0.3064 0.4608 0.052 Uiso 1 1 calc R
H4B H 0.2529 0.3911 0.4732 0.052 Uiso 1 1 calc R
C5 C 0.00047(19) 0.23870(10) 0.43712(12) 0.0391(5) Uani 1 1 d .
H5A H 0.0446 0.2436 0.3998 0.047 Uiso 1 1 calc R
H5B H -0.0847 0.2417 0.4077 0.047 Uiso 1 1 calc R
C6 C 0.02848(16) 0.16720(11) 0.47901(12) 0.0372(5) Uani 1 1 d .
H6A H -0.0221 0.1601 0.5120 0.045 Uiso 1 1 calc R
H6B H 0.0129 0.1277 0.4405 0.045 Uiso 1 1 calc R
C7 C 0.06427(18) 0.13028(10) 0.72023(14) 0.0423(5) Uani 1 1 d .
H7A H 0.0743 0.1150 0.6711 0.063 Uiso 1 1 calc R
H7B H 0.0127 0.0964 0.7348 0.063 Uiso 1 1 calc R
H7C H 0.1411 0.1316 0.7612 0.063 Uiso 1 1 calc R
C8 C -0.16548(18) 0.20987(13) 0.65623(15) 0.0512(6) Uani 1 1 d .
H8A H -0.1775 0.1866 0.6058 0.077 Uiso 1 1 calc R
H8B H -0.2040 0.2568 0.6480 0.077 Uiso 1 1 calc R
H8C H -0.1994 0.1800 0.6880 0.077 Uiso 1 1 calc R
C9 C 0.01846(19) 0.26212(11) 0.80821(13) 0.0399(5) Uani 1 1 d .
C10 C -0.0296(2) 0.33845(12) 0.80109(14) 0.0521(6) Uani 1 1 d .
H10A H -0.0184 0.3579 0.8532 0.078 Uiso 1 1 calc R
H10B H -0.1136 0.3381 0.7710 0.078 Uiso 1 1 calc R
H10C H 0.0126 0.3684 0.7744 0.078 Uiso 1 1 calc R
C11 C -0.0466(3) 0.21647(15) 0.85238(16) 0.0679(8) Uani 1 1 d .
H11A H -0.0333 0.2368 0.9044 0.102 Uiso 1 1 calc R
H11B H -0.0168 0.1672 0.8573 0.102 Uiso 1 1 calc R
H11C H -0.1311 0.2164 0.8235 0.102 Uiso 1 1 calc R
C12 C 0.1500(2) 0.26468(15) 0.85601(15) 0.0624(7) Uani 1 1 d .
H12A H 0.1597 0.2848 0.9076 0.094 Uiso 1 1 calc R
H12B H 0.1915 0.2948 0.8291 0.094 Uiso 1 1 calc R
H12C H 0.1826 0.2161 0.8617 0.094 Uiso 1 1 calc R
C13 C 0.2759(2) 0.49711(11) 0.58363(14) 0.0478(5) Uani 1 1 d .
H13A H 0.1956 0.4991 0.5859 0.072 Uiso 1 1 calc R
H13B H 0.2737 0.5007 0.5292 0.072 Uiso 1 1 calc R
H13C H 0.3219 0.5370 0.6136 0.072 Uiso 1 1 calc R
C14 C 0.34510(19) 0.40794(11) 0.72958(12) 0.0402(5) Uani 1 1 d .
H14A H 0.2652 0.3978 0.7299 0.060 Uiso 1 1 calc R
H14B H 0.3706 0.4546 0.7539 0.060 Uiso 1 1 calc R
H14C H 0.3988 0.3706 0.7588 0.060 Uiso 1 1 calc R
C15 C 0.50388(18) 0.40789(10) 0.62471(12) 0.0379(4) Uani 1 1 d .
C16 C 0.5704(2) 0.47546(13) 0.66431(17) 0.0614(7) Uani 1 1 d .
H16A H 0.6524 0.4728 0.6653 0.092 Uiso 1 1 calc R
H16B H 0.5683 0.4785 0.7178 0.092 Uiso 1 1 calc R
H16C H 0.5329 0.5180 0.6351 0.092 Uiso 1 1 calc R
C17 C 0.5052(2) 0.40384(13) 0.54023(15) 0.0577(6) Uani 1 1 d .
H17A H 0.5866 0.4062 0.5400 0.087 Uiso 1 1 calc R
H17B H 0.4604 0.4441 0.5103 0.087 Uiso 1 1 calc R
H17C H 0.4693 0.3587 0.5166 0.087 Uiso 1 1 calc R
C18 C 0.56874(19) 0.34129(12) 0.66717(14) 0.0476(5) Uani 1 1 d .
H18A H 0.6498 0.3414 0.6660 0.071 Uiso 1 1 calc R
H18B H 0.5282 0.2981 0.6412 0.071 Uiso 1 1 calc R
H18C H 0.5696 0.3419 0.7214 0.071 Uiso 1 1 calc R
C19 C 0.2166(2) 0.13740(14) 0.38572(13) 0.0553(6) Uani 1 1 d .
H19A H 0.2330 0.1879 0.3784 0.083 Uiso 1 1 calc R
H19B H 0.1334 0.1272 0.3582 0.083 Uiso 1 1 calc R
H19C H 0.2658 0.1069 0.3649 0.083 Uiso 1 1 calc R
C20 C 0.40250(18) 0.15138(13) 0.54435(14) 0.0507(6) Uani 1 1 d .
H20A H 0.4033 0.2039 0.5438 0.076 Uiso 1 1 calc R
H20B H 0.4564 0.1331 0.5181 0.076 Uiso 1 1 calc R
H20C H 0.4276 0.1343 0.5984 0.076 Uiso 1 1 calc R
C21 C 0.24019(19) 0.01757(11) 0.50418(14) 0.0441(5) Uani 1 1 d .
C22 C 0.3458(3) -0.02014(16) 0.4919(2) 0.0926(12) Uani 1 1 d .
H22A H 0.3369 -0.0721 0.4955 0.139 Uiso 1 1 calc R
H22B H 0.4182 -0.0046 0.5321 0.139 Uiso 1 1 calc R
H22C H 0.3500 -0.0079 0.4403 0.139 Uiso 1 1 calc R
C23 C 0.1286(2) -0.01246(14) 0.44349(17) 0.0661(7) Uani 1 1 d .
H23A H 0.1262 -0.0646 0.4494 0.099 Uiso 1 1 calc R
H23B H 0.1296 -0.0009 0.3910 0.099 Uiso 1 1 calc R
H23C H 0.0589 0.0090 0.4515 0.099 Uiso 1 1 calc R
C24 C 0.2338(3) -0.00149(14) 0.58497(17) 0.0748(8) Uani 1 1 d .
H24A H 0.2242 -0.0534 0.5884 0.112 Uiso 1 1 calc R
H24B H 0.1665 0.0230 0.5931 0.112 Uiso 1 1 calc R
H24C H 0.3065 0.0137 0.6251 0.112 Uiso 1 1 calc R
C25 C 0.34629(16) 0.21269(10) 0.72518(11) 0.0317(4) Uani 1 1 d .
H25A H 0.4003 0.2543 0.7370 0.038 Uiso 1 1 calc R
H25B H 0.3065 0.2137 0.7652 0.038 Uiso 1 1 calc R
C26 C 0.42757(16) 0.14957(10) 0.74842(10) 0.0297(4) Uani 1 1 d .
C27 C 0.54478(18) 0.15360(12) 0.75169(13) 0.0433(5) Uani 1 1 d .
H27A H 0.5747 0.1977 0.7398 0.052 Uiso 1 1 calc R
C28 C 0.61904(19) 0.09464(13) 0.77200(14) 0.0530(6) Uani 1 1 d .
H28A H 0.6985 0.0989 0.7732 0.064 Uiso 1 1 calc R
C29 C 0.5793(2) 0.03024(12) 0.79031(14) 0.0516(6) Uani 1 1 d .
H29A H 0.6303 -0.0100 0.8043 0.062 Uiso 1 1 calc R
C30 C 0.4644(2) 0.02545(11) 0.78788(15) 0.0514(6) Uani 1 1 d .
H30A H 0.4355 -0.0187 0.8004 0.062 Uiso 1 1 calc R
C31 C 0.38980(17) 0.08390(10) 0.76749(13) 0.0393(5) Uani 1 1 d .
H31A H 0.3106 0.0790 0.7665 0.047 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'
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_publ_flag
N3 Zr1 N2 112.75(6) y
N3 Zr1 N1 112.55(6) y
N2 Zr1 N1 111.12(6) y
N3 Zr1 C25 112.99(6) y
N2 Zr1 C25 104.12(6) y
N1 Zr1 C25 102.57(6) y
N3 Zr1 N4 73.40(6) y
N2 Zr1 N4 73.59(6) y
N1 Zr1 N4 73.07(6) y
C25 Zr1 N4 173.50(6) y
N1 Si1 C7 108.72(9) ?
N1 Si1 C8 110.72(10) ?
C7 Si1 C8 106.95(10) ?
N1 Si1 C9 112.41(9) ?
C7 Si1 C9 109.15(10) ?
C8 Si1 C9 108.73(10) ?
C2 N1 Si1 115.73(13) ?
C2 N1 Zr1 113.62(12) ?
Si1 N1 Zr1 128.43(9) ?
N4 C1 C2 108.27(16) ?
N2 Si2 C14 110.13(8) ?
N2 Si2 C13 110.72(9) ?
C14 Si2 C13 105.89(10) ?
N2 Si2 C15 110.91(8) ?
C14 Si2 C15 110.19(10) ?
C13 Si2 C15 108.88(10) ?
C4 N2 Si2 114.83(12) ?
C4 N2 Zr1 112.52(11) ?
Si2 N2 Zr1 131.28(8) ?
N1 C2 C1 108.60(16) ?
N3 Si3 C20 107.36(9) ?
N3 Si3 C19 110.04(10) ?
C20 Si3 C19 107.98(11) ?
N3 Si3 C21 113.09(8) ?
C20 Si3 C21 110.73(11) ?
C19 Si3 C21 107.54(11) ?
C6 N3 Si3 116.45(12) ?
C6 N3 Zr1 113.82(12) ?
Si3 N3 Zr1 126.87(8) ?
N4 C3 C4 108.23(16) ?
C1 N4 C5 112.12(16) ?
C1 N4 C3 112.22(16) ?
C5 N4 C3 112.11(16) ?
C1 N4 Zr1 106.94(11) ?
C5 N4 Zr1 106.69(11) ?
C3 N4 Zr1 106.29(11) ?
N2 C4 C3 108.47(17) ?
N4 C5 C6 108.40(16) ?
N3 C6 C5 108.98(15) ?
C10 C9 C12 108.0(2) ?
C10 C9 C11 108.55(19) ?
C12 C9 C11 109.0(2) ?
C10 C9 Si1 110.98(15) ?
C12 C9 Si1 110.36(15) ?
C11 C9 Si1 109.88(16) ?
C18 C15 C17 107.02(18) ?
C18 C15 C16 109.07(19) ?
C17 C15 C16 109.48(18) ?
C18 C15 Si2 110.52(14) ?
C17 C15 Si2 110.28(16) ?
C16 C15 Si2 110.40(15) ?
C22 C21 C24 109.4(2) ?
C22 C21 C23 107.4(2) ?
C24 C21 C23 107.3(2) ?
C22 C21 Si3 110.69(17) ?
C24 C21 Si3 111.24(16) ?
C23 C21 Si3 110.60(17) ?
C26 C25 Zr1 134.63(13) ?
C31 C26 C27 116.38(18) ?
C31 C26 C25 121.84(17) ?
C27 C26 C25 121.78(17) ?
C28 C27 C26 121.5(2) ?
C29 C28 C27 120.9(2) ?
C30 C29 C28 118.3(2) ?
C29 C30 C31 121.1(2) ?
C30 C31 C26 121.77(19) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 N3 2.0727(15) y
Zr1 N2 2.0796(15) y
Zr1 N1 2.0885(16) y
Zr1 C25 2.3243(18) y
Zr1 N4 2.5484(15) y
Si1 N1 1.7401(17) ?
Si1 C7 1.870(2) ?
Si1 C8 1.882(2) ?
Si1 C9 1.907(2) ?
N1 C2 1.491(2) ?
C1 N4 1.479(3) ?
C1 C2 1.516(3) ?
Si2 N2 1.7382(16) ?
Si2 C14 1.878(2) ?
Si2 C13 1.889(2) ?
Si2 C15 1.900(2) ?
N2 C4 1.493(2) ?
Si3 N3 1.7404(16) ?
Si3 C20 1.869(2) ?
Si3 C19 1.874(2) ?
Si3 C21 1.906(2) ?
N3 C6 1.489(2) ?
C3 N4 1.484(2) ?
C3 C4 1.521(3) ?
N4 C5 1.481(2) ?
C5 C6 1.518(3) ?
C9 C10 1.526(3) ?
C9 C12 1.537(3) ?
C9 C11 1.544(3) ?
C15 C18 1.535(3) ?
C15 C17 1.539(3) ?
C15 C16 1.540(3) ?
C21 C22 1.528(3) ?
C21 C24 1.533(4) ?
C21 C23 1.538(3) ?
C25 C26 1.501(2) ?
C26 C31 1.389(3) ?
C26 C27 1.391(3) ?
C27 C28 1.389(3) ?
C28 C29 1.373(3) ?
C29 C30 1.369(3) ?
C30 C31 1.384(3) ?
