#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:25:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179789 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/85/7008539.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_7008539
loop_
_publ_author_name
'Wiecko, Michal'
'Girnt, Denise'
'Rastätter, Marcus'
'Panda, Tarun K.'
'Roesky, Peter W.'
_publ_section_title
;
 Zirconium complexes having a chiral phosphanylamide in the
 co-ordination sphere.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2147
_journal_page_last               2150
_journal_paper_doi               10.1039/b503956h
_journal_year                    2005
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C41 H40 N P Zr'
_chemical_formula_weight         668.93
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.067(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.798(2)
_cell_length_b                   9.975(3)
_cell_length_c                   19.110(5)
_cell_measurement_temperature    173(2)
_cell_volume                     1670.5(8)
_computing_molecular_graphics    'Diamond 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       'area detector'
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20675
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.848144
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS - Bruker/Siemens'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         10067
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0246P)²+0.3750P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                7951
_reflns_number_total             10067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503956h.txt
_cod_data_source_block           5
_cod_original_cell_volume        1670.7(7)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7008539
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, 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 1.04804(2) 0.29581(2) 1.218956(12) 0.02384(6) Uani 1 1 d . . .
N N 0.9598(2) 0.4871(2) 1.23584(11) 0.0249(5) Uani 1 1 d . . .
P P 1.13363(8) 0.53289(6) 1.26841(4) 0.02513(14) Uani 1 1 d . . .
C1 C 0.8232(3) 0.5721(3) 1.22334(13) 0.0266(5) Uani 1 1 d . . .
H1 H 0.8457 0.6435 1.1890 0.032 Uiso 1 1 calc R . .
C2 C 0.6900(3) 0.4885(3) 1.19067(17) 0.0341(7) Uani 1 1 d . . .
H2A H 0.7205 0.4428 1.1487 0.051 Uiso 1 1 calc R . .
H2B H 0.6028 0.5473 1.1776 0.051 Uiso 1 1 calc R . .
H2C H 0.6612 0.4218 1.2248 0.051 Uiso 1 1 calc R . .
C3 C 0.7787(3) 0.6398(3) 1.28945(14) 0.0254(5) Uani 1 1 d . . .
C4 C 0.7493(3) 0.7757(3) 1.28989(14) 0.0300(6) Uani 1 1 d . . .
H4 H 0.7595 0.8272 1.2487 0.036 Uiso 1 1 calc R . .
C5 C 0.7049(3) 0.8382(3) 1.34970(16) 0.0373(7) Uani 1 1 d . . .
H5 H 0.6849 0.9318 1.3491 0.045 Uiso 1 1 calc R . .
C6 C 0.6898(3) 0.7654(3) 1.40969(16) 0.0401(8) Uani 1 1 d . . .
H6 H 0.6587 0.8082 1.4505 0.048 Uiso 1 1 calc R . .
C7 C 0.7206(3) 0.6285(3) 1.41027(16) 0.0384(7) Uani 1 1 d . . .
H7 H 0.7125 0.5778 1.4519 0.046 Uiso 1 1 calc R . .
C8 C 0.7629(3) 0.5662(3) 1.35043(14) 0.0317(6) Uani 1 1 d . . .
H8 H 0.7814 0.4724 1.3508 0.038 Uiso 1 1 calc R . .
C9 C 1.1361(3) 0.6060(3) 1.35599(14) 0.0291(6) Uani 1 1 d . . .
C10 C 1.1145(3) 0.7424(3) 1.36694(15) 0.0338(6) Uani 1 1 d . . .
H10 H 1.1057 0.8021 1.3281 0.041 Uiso 1 1 calc R . .
C11 C 1.1060(3) 0.7912(5) 1.43393(14) 0.0436(6) Uani 1 1 d . . .
H11 H 1.0921 0.8845 1.4411 0.052 Uiso 1 1 calc R . .
C12 C 1.1174(4) 0.7058(4) 1.49010(17) 0.0536(9) Uani 1 1 d . . .
H12 H 1.1101 0.7400 1.5361 0.064 Uiso 1 1 calc R . .
C13 C 1.1392(4) 0.5712(4) 1.48052(16) 0.0513(9) Uani 1 1 d . . .
H13 H 1.1472 0.5124 1.5198 0.062 Uiso 1 1 calc R . .
C14 C 1.1495(3) 0.5210(3) 1.41344(15) 0.0395(7) Uani 1 1 d . . .
H14 H 1.1657 0.4278 1.4069 0.047 Uiso 1 1 calc R . .
C15 C 1.2071(3) 0.6622(2) 1.21369(13) 0.0234(5) Uani 1 1 d . . .
C16 C 1.1463(3) 0.6789(3) 1.14488(14) 0.0288(6) Uani 1 1 d . . .
H16 H 1.0594 0.6281 1.1280 0.035 Uiso 1 1 calc R . .
C17 C 1.2100(3) 0.7686(3) 1.10014(14) 0.0343(7) Uani 1 1 d . . .
H17 H 1.1669 0.7791 1.0531 0.041 Uiso 1 1 calc R . .
C18 C 1.3367(3) 0.8422(3) 1.12470(15) 0.0354(7) Uani 1 1 d . . .
H18 H 1.3814 0.9036 1.0945 0.042 Uiso 1 1 calc R . .
C19 C 1.3984(3) 0.8263(3) 1.19342(15) 0.0346(7) Uani 1 1 d . . .
H19 H 1.4849 0.8777 1.2103 0.042 Uiso 1 1 calc R . .
C20 C 1.3358(3) 0.7369(3) 1.23737(15) 0.0304(6) Uani 1 1 d . . .
H20 H 1.3802 0.7258 1.2841 0.036 Uiso 1 1 calc R . .
C21 C 0.9514(3) 0.1664(3) 1.30357(15) 0.0350(7) Uani 1 1 d . . .
H21A H 1.0276 0.1105 1.3314 0.042 Uiso 1 1 calc R . .
H21B H 0.8835 0.2143 1.3338 0.042 Uiso 1 1 calc R . .
C22 C 0.8744(3) 0.1007(3) 1.24329(15) 0.0287(6) Uani 1 1 d . . .
C23 C 0.9523(3) 0.0216(3) 1.19759(16) 0.0348(6) Uani 1 1 d . . .
H23 H 1.0565 0.0001 1.2097 0.042 Uiso 1 1 calc R . .
C24 C 0.8801(4) -0.0262(3) 1.13466(17) 0.0420(8) Uani 1 1 d . . .
H24 H 0.9336 -0.0839 1.1058 0.050 Uiso 1 1 calc R . .
C25 C 0.7325(4) 0.0093(3) 1.11417(17) 0.0434(8) Uani 1 1 d . . .
H25 H 0.6842 -0.0223 1.0709 0.052 Uiso 1 1 calc R . .
C26 C 0.6547(4) 0.0912(3) 1.15674(18) 0.0393(8) Uani 1 1 d . . .
H26 H 0.5528 0.1168 1.1422 0.047 Uiso 1 1 calc R . .
C27 C 0.7220(3) 0.1365(3) 1.21981(16) 0.0333(7) Uani 1 1 d . . .
H27 H 0.6658 0.1927 1.2483 0.040 Uiso 1 1 calc R . .
C28 C 0.9803(3) 0.2977(4) 1.09963(12) 0.0335(5) Uani 1 1 d . . .
H28A H 0.8982 0.2316 1.0877 0.040 Uiso 1 1 calc R . .
H28B H 0.9423 0.3876 1.0848 0.040 Uiso 1 1 calc R . .
C29 C 1.1173(3) 0.2632(3) 1.06307(13) 0.0314(7) Uani 1 1 d . . .
C30 C 1.1294(3) 0.1417(3) 1.02777(14) 0.0348(6) Uani 1 1 d . . .
H30 H 1.0458 0.0812 1.0248 0.042 Uiso 1 1 calc R . .
C31 C 1.2606(4) 0.1075(3) 0.99699(16) 0.0441(8) Uani 1 1 d . . .
H31 H 1.2648 0.0250 0.9724 0.053 Uiso 1 1 calc R . .
C32 C 1.3853(4) 0.1916(4) 1.00151(17) 0.0492(8) Uani 1 1 d . . .
H32 H 1.4756 0.1672 0.9809 0.059 Uiso 1 1 calc R . .
C33 C 1.3766(3) 0.3113(5) 1.03639(15) 0.0458(8) Uani 1 1 d . . .
H33 H 1.4620 0.3699 1.0402 0.055 Uiso 1 1 calc R . .
C34 C 1.2449(4) 0.3474(3) 1.06601(15) 0.0403(7) Uani 1 1 d . . .
H34 H 1.2408 0.4317 1.0890 0.048 Uiso 1 1 calc R . .
C35 C 1.2973(3) 0.2311(3) 1.22854(14) 0.0326(6) Uani 1 1 d . . .
H35A H 1.3062 0.1483 1.2006 0.039 Uiso 1 1 calc R . .
H35B H 1.3578 0.3015 1.2072 0.039 Uiso 1 1 calc R . .
C36 C 1.3666(3) 0.2056(3) 1.30121(14) 0.0291(6) Uani 1 1 d . . .
C37 C 1.4438(3) 0.3055(4) 1.34068(13) 0.0355(6) Uani 1 1 d . . .
H37 H 1.4538 0.3919 1.3207 0.043 Uiso 1 1 calc R . .
C38 C 1.5065(3) 0.2811(5) 1.40874(15) 0.0434(8) Uani 1 1 d . . .
H38 H 1.5601 0.3504 1.4345 0.052 Uiso 1 1 calc R . .
C39 C 1.4916(3) 0.1571(4) 1.43907(17) 0.0463(8) Uani 1 1 d . . .
H39 H 1.5343 0.1407 1.4857 0.056 Uiso 1 1 calc R . .
C40 C 1.4149(3) 0.0581(3) 1.40160(17) 0.0447(8) Uani 1 1 d . . .
H40 H 1.4033 -0.0274 1.4223 0.054 Uiso 1 1 calc R . .
C41 C 1.3539(3) 0.0815(3) 1.33364(17) 0.0384(7) Uani 1 1 d . . .
H41 H 1.3018 0.0109 1.3082 0.046 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'
P P 0.1023 0.0942 '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
N Zr C35 127.79(10) . . ?
N Zr C21 103.81(10) . . ?
C35 Zr C21 101.44(11) . . ?
N Zr C28 94.46(12) . . ?
C35 Zr C28 104.16(9) . . ?
C21 Zr C28 128.57(12) . . ?
N Zr C22 115.59(10) . . ?
C35 Zr C22 110.99(10) . . ?
C21 Zr C22 34.21(10) . . ?
C28 Zr C22 94.61(11) . . ?
N Zr P 39.18(6) . . ?
C35 Zr P 89.01(7) . . ?
C21 Zr P 111.41(8) . . ?
C28 Zr P 112.86(11) . . ?
C22 Zr P 141.23(7) . . ?
C1 N P 127.78(18) . . ?
C1 N Zr 143.83(17) . . ?
P N Zr 88.09(10) . . ?
N P C15 110.01(11) . . ?
N P C9 112.90(12) . . ?
C15 P C9 105.58(12) . . ?
N P Zr 52.73(7) . . ?
C15 P Zr 122.47(8) . . ?
C9 P Zr 131.95(9) . . ?
N C1 C3 112.9(2) . . ?
N C1 C2 109.7(2) . . ?
C3 C1 C2 109.8(2) . . ?
C4 C3 C8 118.6(3) . . ?
C4 C3 C1 120.4(2) . . ?
C8 C3 C1 121.0(2) . . ?
C3 C4 C5 120.8(3) . . ?
C6 C5 C4 120.3(3) . . ?
C5 C6 C7 119.5(3) . . ?
C8 C7 C6 120.1(3) . . ?
C7 C8 C3 120.6(3) . . ?
C14 C9 C10 118.9(3) . . ?
C14 C9 P 118.5(2) . . ?
C10 C9 P 122.5(2) . . ?
C11 C10 C9 120.3(3) . . ?
C12 C11 C10 120.2(4) . . ?
C11 C12 C13 120.4(3) . . ?
C12 C13 C14 119.9(3) . . ?
C9 C14 C13 120.3(3) . . ?
C16 C15 C20 118.5(2) . . ?
C16 C15 P 120.32(19) . . ?
C20 C15 P 120.8(2) . . ?
C15 C16 C17 121.2(2) . . ?
C18 C17 C16 119.4(2) . . ?
C17 C18 C19 119.9(2) . . ?
C20 C19 C18 120.6(3) . . ?
C19 C20 C15 120.4(3) . . ?
C22 C21 Zr 82.49(16) . . ?
C23 C22 C27 116.4(3) . . ?
C23 C22 C21 122.2(3) . . ?
C27 C22 C21 120.1(3) . . ?
C23 C22 Zr 88.98(17) . . ?
C27 C22 Zr 108.39(18) . . ?
C21 C22 Zr 63.30(14) . . ?
C24 C23 C22 121.3(3) . . ?
C25 C24 C23 120.5(3) . . ?
C24 C25 C26 119.5(3) . . ?
C27 C26 C25 121.1(3) . . ?
C26 C27 C22 121.1(3) . . ?
C29 C28 Zr 108.29(16) . . ?
C30 C29 C34 116.5(3) . . ?
C30 C29 C28 121.9(3) . . ?
C34 C29 C28 121.5(3) . . ?
C31 C30 C29 121.4(3) . . ?
C32 C31 C30 120.8(3) . . ?
C33 C32 C31 118.8(3) . . ?
C32 C33 C34 120.7(3) . . ?
C33 C34 C29 121.7(3) . . ?
C36 C35 Zr 115.82(18) . . ?
C37 C36 C41 116.7(3) . . ?
C37 C36 C35 121.6(3) . . ?
C41 C36 C35 121.6(3) . . ?
C38 C37 C36 121.2(4) . . ?
C39 C38 C37 120.4(4) . . ?
C40 C39 C38 119.4(3) . . ?
C39 C40 C41 120.3(3) . . ?
C40 C41 C36 121.9(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 N 2.096(2) . ?
Zr C35 2.278(3) . ?
Zr C21 2.290(3) . ?
Zr C28 2.305(2) . ?
Zr C22 2.542(3) . ?
Zr P 2.6319(9) . ?
N C1 1.473(3) . ?
N P 1.664(2) . ?
P C15 1.815(3) . ?
P C9 1.824(3) . ?
C1 C3 1.514(4) . ?
C1 C2 1.526(4) . ?
C3 C4 1.381(4) . ?
C3 C8 1.395(4) . ?
C4 C5 1.388(4) . ?
C5 C6 1.373(4) . ?
C6 C7 1.393(4) . ?
C7 C8 1.381(4) . ?
C9 C14 1.384(4) . ?
C9 C10 1.392(4) . ?
C10 C11 1.378(4) . ?
C11 C12 1.367(5) . ?
C12 C13 1.371(5) . ?
C13 C14 1.387(5) . ?
C15 C16 1.385(4) . ?
C15 C20 1.396(4) . ?
C16 C17 1.389(4) . ?
C17 C18 1.382(4) . ?
C18 C19 1.385(4) . ?
C19 C20 1.373(4) . ?
C21 C22 1.441(4) . ?
C22 C23 1.400(4) . ?
C22 C27 1.422(4) . ?
C23 C24 1.394(4) . ?
C24 C25 1.369(5) . ?
C25 C26 1.377(5) . ?
C26 C27 1.372(4) . ?
C28 C29 1.486(4) . ?
C29 C30 1.396(4) . ?
C29 C34 1.399(4) . ?
C30 C31 1.384(4) . ?
C31 C32 1.377(5) . ?
C32 C33 1.372(5) . ?
C33 C34 1.382(4) . ?
C35 C36 1.488(4) . ?
C36 C37 1.390(4) . ?
C36 C41 1.393(4) . ?
C37 C38 1.389(4) . ?
C38 C39 1.377(6) . ?
C39 C40 1.363(5) . ?
C40 C41 1.380(4) . ?
