#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:17:41 +0100 (vie 25 de mar de 2016) $
#$Revision: 179808 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/04/7010449.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_7010449
loop_
_publ_author_name
'Sarsfield, Mark J.'
'Said, Musa'
'Thornton-Pett, Mark'
'Gerrard, Lee A.'
'Bochmann, Manfred'
_publ_section_title
;
 The reactivity of trimethylsilyliminophosphines towards titanium and
 zirconium halides
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              822
_journal_paper_doi               10.1039/b009082o
_journal_year                    2001
_chemical_formula_moiety         'Zr2 Si2 C52 H66 Cl10 N2 P2'
_chemical_formula_sum            'C52 H66 Cl10 N2 P2 Si2 Zr2'
_chemical_formula_weight         1374.13
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.729(3)
_cell_length_b                   11.509(2)
_cell_length_c                   17.448(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3325.6(12)
_computing_cell_refinement
;
DENZO AND SCALEPACK (Otwinowski and Minor, 1985)
;
_computing_data_collection       'MSC Raxis II control software'
_computing_data_reduction        'SHELX97-SHELXPRO (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL+XP
_computing_publication_material  SHELXTL+XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku R-axis IIc'
_diffrn_measurement_method       'image plate oscillation photographs'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9122
_diffrn_reflns_theta_max         25.55
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1400
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   0.994
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_restrained_S_obs      0.994
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_obs          0.0544
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1393P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2193
_refine_ls_wR_factor_obs         0.1653
_reflns_number_observed          3623
_reflns_number_total             5572
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b009082o.txt
_cod_data_source_block           musa1
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1393P)^2^+0.0000P] 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^)+(0.1393P)^2^+0.0000P] 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        3325.5(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010449
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zr1 Zr 0.41258(4) 0.45114(4) 0.06524(3) 0.0689(3) Uani 1 d . .
Cl1 Cl 0.33226(11) 0.3957(2) -0.05643(9) 0.0874(5) Uani 1 d . .
Cl2 Cl 0.38363(14) 0.26706(14) 0.11815(10) 0.0947(6) Uani 1 d . .
Cl3 Cl 0.46168(10) 0.63118(11) -0.00679(9) 0.0732(4) Uani 1 d . .
Cl4 Cl 0.50577(14) 0.5008(2) 0.17852(10) 0.1009(6) Uani 1 d . .
Cl5 Cl 0.30660(14) 0.5649(2) 0.10288(12) 0.1018(6) Uani 1 d . .
P1 P 0.26517(9) 0.97301(14) -0.03510(8) 0.0653(4) Uani 1 d . .
Si1 Si 0.13549(13) 1.1639(2) -0.07587(13) 0.0976(7) Uani 1 d . .
N1 N 0.2334(3) 1.1019(5) -0.0647(3) 0.0738(13) Uani 1 d . .
H1 H 0.2704(3) 1.1472(5) -0.0770(3) 0.089 Uiso 1 calc R .
C1 C 0.3745(4) 0.9732(6) -0.0080(3) 0.0699(14) Uani 1 d . .
C2 C 0.4181(3) 1.0084(5) -0.0764(3) 0.0624(12) Uani 1 d . .
C3 C 0.4379(4) 0.9276(5) -0.1278(3) 0.0674(14) Uani 1 d . .
H3 H 0.4237(4) 0.8503(5) -0.1221(3) 0.081 Uiso 1 calc R .
C4 C 0.4790(4) 0.9589(5) -0.1884(4) 0.0703(15) Uani 1 d . .
H4 H 0.4931(4) 0.9012(5) -0.2213(4) 0.084 Uiso 1 calc R .
C5 C 0.4993(4) 1.0713(5) -0.2015(3) 0.0672(14) Uani 1 d . .
C6 C 0.4769(4) 1.1569(5) -0.1502(4) 0.0714(15) Uani 1 d . .
H6 H 0.4898(4) 1.2345(5) -0.1572(4) 0.086 Uiso 1 calc R .
C7 C 0.4361(4) 1.1255(5) -0.0900(3) 0.0708(15) Uani 1 d . .
H7 H 0.4201(4) 1.1828(5) -0.0578(3) 0.085 Uiso 1 calc R .
C8 C 0.5431(5) 1.1061(7) -0.2703(4) 0.091(2) Uani 1 d . .
C9 C 0.4866(9) 1.1664(27) -0.3301(9) 0.437(22) Uani 1 d . .
H9A H 0.5144(9) 1.1875(27) -0.3725(9) 0.656 Uiso 1 calc R .
H9B H 0.4664(9) 1.2351(27) -0.3083(9) 0.656 Uiso 1 calc R .
H9C H 0.4424(9) 1.1156(27) -0.3483(9) 0.656 Uiso 1 calc R .
C10 C 0.5852(7) 0.9971(10) -0.3014(7) 0.164(5) Uani 1 d . .
H10A H 0.6208(7) 0.9623(10) -0.2598(7) 0.246 Uiso 1 calc R .
H10B H 0.6155(7) 1.0208(10) -0.3415(7) 0.246 Uiso 1 calc R .
H10C H 0.5449(7) 0.9417(10) -0.3219(7) 0.246 Uiso 1 calc R .
C11 C 0.6158(9) 1.1939(12) -0.2395(8) 0.215(9) Uani 1 d . .
H11A H 0.6531(9) 1.1559(12) -0.2006(8) 0.323 Uiso 1 calc R .
H11B H 0.5943(9) 1.2617(12) -0.2178(8) 0.323 Uiso 1 calc R .
H11C H 0.6434(9) 1.2163(12) -0.2819(8) 0.323 Uiso 1 calc R .
C12 C 0.2416(3) 0.8655(5) -0.1091(3) 0.0646(13) Uani 1 d . .
C13 C 0.2033(4) 0.8960(6) -0.1812(4) 0.079(2) Uani 1 d . .
H13 H 0.1876(4) 0.9725(6) -0.1920(4) 0.095 Uiso 1 calc R .
C14 C 0.1884(4) 0.8093(8) -0.2385(4) 0.095(2) Uani 1 d . .
H14 H 0.1623(4) 0.8288(8) -0.2875(4) 0.114 Uiso 1 calc R .
C15 C 0.2123(5) 0.6944(7) -0.2226(5) 0.094(2) Uani 1 d . .
H15 H 0.2008(5) 0.6371(7) -0.2602(5) 0.113 Uiso 1 calc R .
C16 C 0.2515(4) 0.6680(6) -0.1537(4) 0.084(2) Uani 1 d . .
H16 H 0.2695(4) 0.5922(6) -0.1440(4) 0.101 Uiso 1 calc R .
C17 C 0.2663(4) 0.7501(6) -0.0953(4) 0.077(2) Uani 1 d . .
H17 H 0.2928(4) 0.7286(6) -0.0469(4) 0.092 Uiso 1 calc R .
C18 C 0.2202(4) 0.9353(6) 0.0487(4) 0.073(2) Uani 1 d . .
C19 C 0.2278(5) 1.0184(8) 0.1102(4) 0.097(2) Uani 1 d . .
H19 H 0.2553(5) 1.0878(8) 0.1058(4) 0.117 Uiso 1 calc R .
C20 C 0.1939(6) 0.9947(12) 0.1765(5) 0.129(3) Uani 1 d . .
H20 H 0.1956(6) 1.0502(12) 0.2155(5) 0.154 Uiso 1 calc R .
C21 C 0.1584(6) 0.8911(12) 0.1845(5) 0.124(3) Uani 1 d . .
H21 H 0.1392(6) 0.8752(12) 0.2309(5) 0.148 Uiso 1 calc R .
C22 C 0.1486(6) 0.8039(10) 0.1251(6) 0.124(3) Uani 1 d . .
H22 H 0.1222(6) 0.7341(10) 0.1310(6) 0.149 Uiso 1 calc R .
C23 C 0.1819(5) 0.8310(7) 0.0567(5) 0.102(2) Uani 1 d . .
H23 H 0.1778(5) 0.7772(7) 0.0165(5) 0.122 Uiso 1 calc R .
C24 C 0.0616(5) 1.0461(10) -0.0770(7) 0.161(6) Uani 1 d . .
H24A H 0.0705(5) 1.0051(10) -0.0287(7) 0.242 Uiso 1 calc R .
H24B H 0.0675(5) 0.9934(10) -0.1186(7) 0.242 Uiso 1 calc R .
H24C H 0.0080(5) 1.0780(10) -0.0845(7) 0.242 Uiso 1 calc R .
C25 C 0.1213(6) 1.2453(8) -0.1670(5) 0.117(3) Uani 1 d . .
H25A H 0.1607(6) 1.3062(8) -0.1648(5) 0.175 Uiso 1 calc R .
H25B H 0.0681(6) 1.2784(8) -0.1750(5) 0.175 Uiso 1 calc R .
H25C H 0.1276(6) 1.1938(8) -0.2091(5) 0.175 Uiso 1 calc R .
C26 C 0.1291(9) 1.2617(12) 0.0067(7) 0.206(7) Uani 1 d . .
H26A H 0.1367(9) 1.2177(12) 0.0539(7) 0.310 Uiso 1 calc R .
H26B H 0.0770(9) 1.2982(12) 0.0006(7) 0.310 Uiso 1 calc R .
H26C H 0.1703(9) 1.3201(12) 0.0086(7) 0.310 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'
P P 0.1023 0.0942 '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
Cl5 Zr1 Cl2 100.51(7) . . ?
Cl5 Zr1 Cl4 93.68(8) . . ?
Cl2 Zr1 Cl4 92.09(7) . . ?
Cl5 Zr1 Cl1 92.54(8) . . ?
Cl2 Zr1 Cl1 89.28(7) . . ?
Cl4 Zr1 Cl1 173.28(7) . . ?
Cl5 Zr1 Cl3 89.62(6) . . ?
Cl2 Zr1 Cl3 169.56(6) . . ?
Cl4 Zr1 Cl3 89.74(6) . . ?
Cl1 Zr1 Cl3 87.75(6) . . ?
Cl5 Zr1 Cl3 166.74(6) . 3_665 ?
Cl2 Zr1 Cl3 92.71(6) . 3_665 ?
Cl4 Zr1 Cl3 86.76(7) . 3_665 ?
Cl1 Zr1 Cl3 86.60(6) . 3_665 ?
Cl3 Zr1 Cl3 77.12(5) . 3_665 ?
Zr1 Cl3 Zr1 102.88(5) . 3_665 ?
N1 P1 C18 108.8(3) . . ?
N1 P1 C12 111.7(3) . . ?
C18 P1 C12 110.3(3) . . ?
N1 P1 C1 110.5(3) . . ?
C18 P1 C1 108.1(3) . . ?
C12 P1 C1 107.3(3) . . ?
N1 Si1 C25 107.8(3) . . ?
N1 Si1 C24 108.4(3) . . ?
C25 Si1 C24 111.3(5) . . ?
N1 Si1 C26 108.4(5) . . ?
C25 Si1 C26 110.6(5) . . ?
C24 Si1 C26 110.3(6) . . ?
P1 N1 Si1 130.8(3) . . ?
C2 C1 P1 111.6(4) . . ?
C3 C2 C7 117.7(5) . . ?
C3 C2 C1 121.1(5) . . ?
C7 C2 C1 121.2(5) . . ?
C2 C3 C4 121.1(5) . . ?
C5 C4 C3 122.4(5) . . ?
C4 C5 C6 117.3(5) . . ?
C4 C5 C8 122.1(5) . . ?
C6 C5 C8 120.5(5) . . ?
C7 C6 C5 120.2(5) . . ?
C6 C7 C2 121.3(5) . . ?
C9 C8 C5 110.2(7) . . ?
C9 C8 C10 113.8(12) . . ?
C5 C8 C10 110.2(6) . . ?
C9 C8 C11 108.5(14) . . ?
C5 C8 C11 108.7(6) . . ?
C10 C8 C11 105.1(8) . . ?
C13 C12 C17 119.2(6) . . ?
C13 C12 P1 120.6(5) . . ?
C17 C12 P1 120.1(5) . . ?
C12 C13 C14 118.8(7) . . ?
C15 C14 C13 120.8(7) . . ?
C16 C15 C14 119.3(7) . . ?
C15 C16 C17 121.8(7) . . ?
C16 C17 C12 120.2(6) . . ?
C23 C18 C19 120.1(6) . . ?
C23 C18 P1 123.3(6) . . ?
C19 C18 P1 116.6(5) . . ?
C20 C19 C18 119.4(9) . . ?
C21 C20 C19 119.9(10) . . ?
C20 C21 C22 123.4(8) . . ?
C23 C22 C21 115.8(9) . . ?
C18 C23 C22 121.2(9) . . ?
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
Zr1 Cl5 2.371(2) . ?
Zr1 Cl2 2.388(2) . ?
Zr1 Cl4 2.407(2) . ?
Zr1 Cl1 2.431(2) . ?
Zr1 Cl3 2.615(2) . ?
Zr1 Cl3 2.640(2) 3_665 ?
Cl3 Zr1 2.640(2) 3_665 ?
P1 N1 1.635(5) . ?
P1 C18 1.790(6) . ?
P1 C12 1.792(6) . ?
P1 C1 1.823(6) . ?
Si1 N1 1.772(5) . ?
Si1 C25 1.832(8) . ?
Si1 C24 1.833(12) . ?
Si1 C26 1.843(11) . ?
C1 C2 1.539(7) . ?
C2 C3 1.365(8) . ?
C2 C7 1.408(8) . ?
C3 C4 1.387(8) . ?
C4 C5 1.366(8) . ?
C5 C6 1.416(8) . ?
C5 C8 1.545(8) . ?
C6 C7 1.380(8) . ?
C8 C9 1.48(2) . ?
C8 C10 1.572(13) . ?
C8 C11 1.614(14) . ?
C12 C13 1.374(8) . ?
C12 C17 1.401(8) . ?
C13 C14 1.411(10) . ?
C14 C15 1.398(11) . ?
C15 C16 1.322(10) . ?
C16 C17 1.385(10) . ?
C18 C23 1.377(10) . ?
C18 C19 1.429(10) . ?
C19 C20 1.386(10) . ?
C20 C21 1.35(2) . ?
C21 C22 1.43(2) . ?
C22 C23 1.422(10) . ?
