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#$Date: 2019-01-11 03:28:24 +0200 (Fri, 11 Jan 2019) $
#$Revision: 212970 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/85/7048577.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_7048577
loop_
_publ_author_name
'Sun, Ziyue'
'Zhao, Yanxia'
'Prior, Timothy J.'
'Elsegood, Mark R. J.'
'Wang, Kuiyuan'
'Xing, Tian'
'Redshaw, Carl'
_publ_section_title
;
 Mono-oxo molybdenum(vi) and tungsten(vi) complexes bearing chelating
 aryloxides: synthesis, structure and ring opening polymerization of
 cyclic esters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT04566F
_journal_year                    2019
_chemical_formula_moiety         'C46 H55 N O5 W'
_chemical_formula_sum            'C46 H55 N O5 W'
_chemical_formula_weight         885.76
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-08-10 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.76192(10)
_cell_length_b                   12.76192(10)
_cell_length_c                   12.52433(18)
_cell_measurement_reflns_used    38670
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.95
_cell_measurement_theta_min      2.22
_cell_volume                     2039.80(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0075
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            92458
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         1.596
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.877
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2357
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0421P)²+4.3390P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2357
_reflns_number_total             2357
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04566f2.cif
_cod_data_source_block           8
_cod_database_code               7048577
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.972
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
W1 W 0.250000 0.250000 0.41880(2) 0.01316(9) Uani 1 4 d S T P
O1 O 0.31658(18) 0.38185(18) 0.44497(18) 0.0084(4) Uani 1 1 d . . .
C1 C 0.3432(2) 0.4341(2) 0.5367(2) 0.0073(6) Uani 1 1 d . U .
C2 C 0.2708(2) 0.5031(2) 0.5810(2) 0.0066(7) Uani 1 1 d . U .
C3 C 0.3007(2) 0.5566(2) 0.6732(2) 0.0085(6) Uani 1 1 d . U .
H3 H 0.252265 0.603700 0.704972 0.010 Uiso 1 1 calc R U .
C4 C 0.3984(2) 0.5439(2) 0.7205(3) 0.0090(6) Uani 1 1 d . U .
C5 C 0.4670(3) 0.4731(3) 0.6739(2) 0.0084(5) Uani 1 1 d . U .
H5 H 0.533795 0.462426 0.705659 0.010 Uiso 1 1 calc R U .
C6 C 0.4411(2) 0.4169(2) 0.5817(2) 0.0071(7) Uani 1 1 d . U .
C7 C 0.4266(3) 0.6105(3) 0.8187(3) 0.0144(6) Uani 1 1 d . U .
C8 C 0.4260(3) 0.7272(3) 0.7868(3) 0.0218(8) Uani 1 1 d . U .
H8A H 0.440456 0.770344 0.849843 0.033 Uiso 1 1 calc R U .
H8B H 0.357234 0.745660 0.757629 0.033 Uiso 1 1 calc R U .
H8C H 0.480079 0.739666 0.732712 0.033 Uiso 1 1 calc R U .
C9 C 0.3453(4) 0.5921(4) 0.9059(3) 0.0241(8) Uani 1 1 d . U .
H9A H 0.346816 0.518297 0.927631 0.036 Uiso 1 1 calc R U .
H9B H 0.275469 0.609491 0.878568 0.036 Uiso 1 1 calc R U .
H9C H 0.361265 0.636526 0.967593 0.036 Uiso 1 1 calc R U .
C10 C 0.5347(3) 0.5848(4) 0.8628(3) 0.0244(8) Uani 1 1 d . U .
H10A H 0.551553 0.633239 0.920989 0.037 Uiso 1 1 calc R U .
H10B H 0.586886 0.591901 0.805852 0.037 Uiso 1 1 calc R U .
H10C H 0.535157 0.512748 0.889779 0.037 Uiso 1 1 calc R U .
C11 C 0.5173(2) 0.3377(2) 0.5352(3) 0.0084(6) Uani 1 1 d . U .
H11A H 0.507669 0.334744 0.456783 0.010 Uiso 1 1 calc R U .
H11B H 0.589863 0.361529 0.549292 0.010 Uiso 1 1 calc R U .
O2 O 0.250000 0.250000 0.2829(3) 0.0223(9) Uani 1 4 d S T P
N1 N 0.250000 0.250000 0.6114(4) 0.0126(8) Uani 1 4 d S TU P
C12 C 0.250000 0.250000 0.6994(6) 0.0285(14) Uani 1 4 d S TU P
C13 C 0.239(14) 0.218(5) 0.8134(12) 0.062(15) Uani 0.25 1 d . U P
H13A H 0.202949 0.273400 0.853179 0.093 Uiso 0.25 1 calc R U P
H13B H 0.308771 0.206693 0.844249 0.093 Uiso 0.25 1 calc R U P
H13C H 0.198479 0.153016 0.817692 0.093 Uiso 0.25 1 calc R U P
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
O1 W1 O1 88.32(2) 2 4
O1 W1 O1 160.27(13) 4 3
O2 W1 O1 99.87(7) . .
O1 W1 O1 160.27(13) 2 .
O2 W1 N1 180.0 . .
O1 W1 N1 80.13(7) . .
C1 O1 W1 132.93(19) . .
O1 C1 C6 119.1(3) . .
O1 C1 C2 118.5(3) . .
C6 C1 C2 122.4(3) . .
C1 C2 C3 117.3(3) . .
C1 C2 C11 122.3(3) . 3
C3 C2 C11 120.4(3) . 3
C4 C3 C2 122.8(3) . .
C4 C3 H3 118.6 . .
C2 C3 H3 118.6 . .
C5 C4 C3 117.6(3) . .
C5 C4 C7 123.2(3) . .
C3 C4 C7 119.1(3) . .
C4 C5 C6 122.1(3) . .
C4 C5 H5 119.0 . .
C6 C5 H5 119.0 . .
C1 C6 C5 117.8(3) . .
C1 C6 C11 121.7(3) . .
C5 C6 C11 120.4(3) . .
C10 C7 C9 108.9(3) . .
C10 C7 C4 112.5(3) . .
C9 C7 C4 109.2(3) . .
C10 C7 C8 107.8(3) . .
C9 C7 C8 109.4(3) . .
C4 C7 C8 108.9(3) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C2 C11 C6 112.8(3) 4 .
C2 C11 H11A 109.0 4 .
C6 C11 H11A 109.0 . .
C2 C11 H11B 109.0 4 .
C6 C11 H11B 109.0 . .
H11A C11 H11B 107.8 . .
C12 N1 W1 180.0 . .
N1 C12 C13 163.2(17) . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O2 1.702(4) .
W1 O1 1.913(2) .
W1 N1 2.412(5) .
O1 C1 1.371(4) .
C1 C6 1.388(4) .
C1 C2 1.391(4) .
C2 C3 1.395(4) .
C2 C11 1.510(4) 3
C3 C4 1.389(4) .
C3 H3 0.9500 .
C4 C5 1.388(5) .
C4 C7 1.538(4) .
C5 C6 1.399(4) .
C5 H5 0.9500 .
C6 C11 1.519(4) .
C7 C10 1.521(5) .
C7 C9 1.525(5) .
C7 C8 1.542(5) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
N1 C12 1.102(9) .
C12 C13 1.49(2) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
W1 O1 C1 C6 89.9(3) . .
W1 O1 C1 C2 -90.5(3) . .
O1 C1 C2 C3 -178.8(3) . .
C6 C1 C2 C3 0.8(4) . .
O1 C1 C2 C11 3.7(4) . 3
C6 C1 C2 C11 -176.7(3) . 3
C1 C2 C3 C4 0.5(5) . .
C11 C2 C3 C4 178.0(3) 3 .
C2 C3 C4 C5 -1.3(5) . .
C2 C3 C4 C7 176.9(3) . .
C3 C4 C5 C6 1.0(4) . .
C7 C4 C5 C6 -177.1(3) . .
O1 C1 C6 C5 178.6(3) . .
C2 C1 C6 C5 -1.0(4) . .
O1 C1 C6 C11 -3.2(4) . .
C2 C1 C6 C11 177.2(3) . .
C4 C5 C6 C1 0.1(4) . .
C4 C5 C6 C11 -178.2(3) . .
C5 C4 C7 C10 -3.7(5) . .
C3 C4 C7 C10 178.2(3) . .
C5 C4 C7 C9 -124.8(4) . .
C3 C4 C7 C9 57.2(4) . .
C5 C4 C7 C8 115.9(4) . .
C3 C4 C7 C8 -62.2(4) . .
C1 C6 C11 C2 -89.0(3) . 4
C5 C6 C11 C2 89.2(3) . 4
