#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:57:43 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263786 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/67/7706768.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_7706768
loop_
_publ_author_name
'Smith, Danielle E.'
'Levason, William'
'Powell, James'
'Reid, Gillian'
_publ_section_title
;
 Synthesis, properties and structural features of molybdenum(v) oxide
 trichloride complexes with neutral chalcogenoether ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4380
_journal_page_last               4389
_journal_paper_doi               10.1039/d1dt00038a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C6 H16 Cl3 Mo O P2'
_chemical_formula_sum            'C6 H16 Cl3 Mo O P2'
_chemical_formula_weight         368.42
_chemical_name_systematic        MoOCl3(dmpe)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.989(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.37160(10)
_cell_length_b                   29.8674(6)
_cell_length_c                   12.4489(2)
_cell_measurement_reflns_used    30241
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.8010
_cell_measurement_theta_min      2.1310
_cell_volume                     2734.24(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.787
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00  21.32   0.38    1.07    --   -8.30 -60.00  30.00  314
  2  ω    -98.00  20.18   0.38    1.07    --   -8.30 -57.00 150.00  311
  3  ω    -98.00  21.32   0.38    1.07    --   -8.30 -60.00 -90.00  314
  4  ω    -98.00  80.22   0.38    1.07    --   -8.30   0.00   0.00  469
  5  ω    -39.00  43.08   0.38    1.07    --   -8.30  38.00  30.00  216
  6  ω    -38.00  80.18   0.38    1.07    --   -8.30  57.00 120.00  311
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0041237000
_diffrn_orient_matrix_UB_12      -0.0039418000
_diffrn_orient_matrix_UB_13      0.0559725000
_diffrn_orient_matrix_UB_21      0.0846703000
_diffrn_orient_matrix_UB_22      -0.0113518000
_diffrn_orient_matrix_UB_23      0.0010796000
_diffrn_orient_matrix_UB_31      0.0460551000
_diffrn_orient_matrix_UB_32      0.0204752000
_diffrn_orient_matrix_UB_33      0.0113462000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.787
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24936
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.852
_diffrn_reflns_theta_min         2.133
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.853
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0616P)²+4.7250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7053
_reflns_number_total             8018
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00038a2.cif
_cod_data_source_block           moocl3dmpe
_cod_depositor_comments
'Adding full bibliography for 7706761--7706769.cif.'
_cod_database_code               7706768
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MoOCl3P2C6H9
_chemical_oxdiff_usercomment     'Yellow Block'
_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.
;
_reflns_odcompleteness_completeness 96.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00G(H00D,H00E), C00H(H00F,H00G), C00I(H00Q,H00R), C00J(H00S,H00T)
2.b Idealised Me refined as rotating group:
 C00F(H00A,H00B,H00C), C00K(H00U,H00V,H00W), C00L(H00H,H00I,H00J), C00M(H00K,
 H00L,H00M), C00N(H00X,H00Y,H), C00O(H00Z,HA,HB), C00P(H00,HC,HD), C00Q(H00N,
 H00O,H00P)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.134
_oxdiff_exptl_absorpt_empirical_full_min 0.571
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo2 Mo 0.53671(3) 0.56966(2) 0.27879(2) 0.01293(7) Uani 1 1 d . . . . .
Mo1 Mo 0.09766(3) 0.69929(2) 0.73630(2) 0.01385(7) Uani 1 1 d . . . . .
Cl5 Cl 0.67718(9) 0.51686(2) 0.15010(5) 0.01634(13) Uani 1 1 d . . . . .
Cl6 Cl 0.68363(9) 0.52869(3) 0.42237(6) 0.01923(14) Uani 1 1 d . . . . .
Cl3 Cl 0.37835(9) 0.65222(3) 0.73692(6) 0.02083(15) Uani 1 1 d . . . . .
P4 P 0.29901(9) 0.50918(2) 0.25203(6) 0.01238(13) Uani 1 1 d . . . . .
Cl4 Cl 0.77757(10) 0.62088(3) 0.24815(6) 0.02151(15) Uani 1 1 d . . . . .
P2 P 0.01628(9) 0.65108(2) 0.57342(6) 0.01377(14) Uani 1 1 d . . . . .
P3 P 0.36375(10) 0.59513(2) 0.10597(6) 0.01499(14) Uani 1 1 d . . . . .
Cl1 Cl 0.23636(10) 0.74178(3) 0.88172(6) 0.02577(16) Uani 1 1 d . . . . .
P1 P 0.28312(9) 0.73585(3) 0.59739(6) 0.01518(14) Uani 1 1 d . . . . .
Cl2 Cl -0.03565(11) 0.64350(3) 0.84279(7) 0.02632(17) Uani 1 1 d . . . . .
O2 O 0.3920(3) 0.60123(8) 0.34543(18) 0.0205(4) Uani 1 1 d . . . . .
O1 O -0.0755(3) 0.73342(8) 0.6967(2) 0.0216(4) Uani 1 1 d . . . . .
C00F C 0.1073(4) 0.51980(11) 0.3305(2) 0.0185(5) Uani 1 1 d . . . . .
H00A H 0.143969 0.516771 0.405675 0.028 Uiso 1 1 calc GR . . . .
H00B H 0.012418 0.498674 0.311182 0.028 Uiso 1 1 calc GR . . . .
H00C H 0.063205 0.549632 0.316521 0.028 Uiso 1 1 calc GR . . . .
C00G C 0.1658(4) 0.55855(11) 0.0766(3) 0.0201(6) Uani 1 1 d . . . . .
H00D H 0.063521 0.569916 0.113375 0.024 Uiso 1 1 calc R . . . .
H00E H 0.132554 0.558971 -0.000117 0.024 Uiso 1 1 calc R . . . .
C00H C 0.2055(4) 0.51039(10) 0.1126(2) 0.0167(5) Uani 1 1 d . . . . .
H00F H 0.291540 0.497005 0.066557 0.020 Uiso 1 1 calc R . . . .
H00G H 0.094200 0.492995 0.105702 0.020 Uiso 1 1 calc R . . . .
C00I C 0.1135(4) 0.67570(10) 0.4551(2) 0.0171(5) Uani 1 1 d . . . . .
H00Q H 0.125517 0.652715 0.400998 0.020 Uiso 1 1 calc R . . . .
H00R H 0.032160 0.698602 0.424431 0.020 Uiso 1 1 calc R . . . .
C00J C 0.3009(4) 0.69644(10) 0.4858(3) 0.0180(5) Uani 1 1 d . . . . .
H00S H 0.344473 0.711964 0.424155 0.022 Uiso 1 1 calc R . . . .
H00T H 0.387167 0.673003 0.506927 0.022 Uiso 1 1 calc R . . . .
C00K C -0.2272(4) 0.64976(11) 0.5431(3) 0.0203(6) Uani 1 1 d . . . . .
H00U H -0.285764 0.640012 0.605496 0.030 Uiso 1 1 calc GR . . . .
H00V H -0.255651 0.629381 0.484708 0.030 Uiso 1 1 calc GR . . . .
H00W H -0.269371 0.679199 0.522954 0.030 Uiso 1 1 calc GR . . . .
C00L C 0.4881(5) 0.59626(11) -0.0134(2) 0.0215(6) Uani 1 1 d . . . . .
H00H H 0.598549 0.612915 0.000675 0.032 Uiso 1 1 calc GR . . . .
H00I H 0.415280 0.610254 -0.070884 0.032 Uiso 1 1 calc GR . . . .
H00J H 0.516720 0.566195 -0.033637 0.032 Uiso 1 1 calc GR . . . .
C00M C 0.3677(4) 0.45213(10) 0.2815(2) 0.0185(5) Uani 1 1 d . . . . .
H00K H 0.475050 0.445294 0.245206 0.028 Uiso 1 1 calc GR . . . .
H00L H 0.271621 0.432094 0.257188 0.028 Uiso 1 1 calc GR . . . .
H00M H 0.392954 0.448705 0.357752 0.028 Uiso 1 1 calc GR . . . .
C00N C 0.5096(4) 0.75276(12) 0.6449(3) 0.0241(6) Uani 1 1 d . . . . .
H00X H 0.502638 0.777801 0.692816 0.036 Uiso 1 1 calc GR . . . .
H00Y H 0.576824 0.761185 0.584749 0.036 Uiso 1 1 calc GR . . . .
H H 0.569927 0.728295 0.682520 0.036 Uiso 1 1 calc GR . . . .
C00O C 0.0888(5) 0.59323(10) 0.5808(3) 0.0234(6) Uani 1 1 d . . . . .
H00Z H 0.216062 0.591463 0.569309 0.035 Uiso 1 1 calc GR . . . .
HA H 0.020815 0.576154 0.526526 0.035 Uiso 1 1 calc GR . . . .
HB H 0.068156 0.581379 0.650619 0.035 Uiso 1 1 calc GR . . . .
C00P C 0.1823(5) 0.78589(11) 0.5372(3) 0.0258(7) Uani 1 1 d . . . . .
H00 H 0.064340 0.778897 0.503790 0.039 Uiso 1 1 calc GR . . . .
HC H 0.258495 0.797183 0.483866 0.039 Uiso 1 1 calc GR . . . .
HD H 0.170420 0.808151 0.591857 0.039 Uiso 1 1 calc GR . . . .
C00Q C 0.2666(5) 0.65021(11) 0.1194(3) 0.0235(6) Uani 1 1 d . . . . .
H00N H 0.186533 0.650059 0.177049 0.035 Uiso 1 1 calc GR . . . .
H00O H 0.199363 0.658266 0.053430 0.035 Uiso 1 1 calc GR . . . .
H00P H 0.362143 0.671562 0.134932 0.035 Uiso 1 1 calc GR . . . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'
P P 0.1023 0.0942 '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 Mo2 P4 77.31(2) . . ?
Cl5 Mo2 P3 81.56(2) . . ?
Cl6 Mo2 Cl5 88.28(3) . . ?
Cl6 Mo2 P4 90.38(3) . . ?
Cl6 Mo2 Cl4 98.35(3) . . ?
Cl6 Mo2 P3 166.27(3) . . ?
P4 Mo2 P3 78.43(2) . . ?
Cl4 Mo2 Cl5 87.51(3) . . ?
Cl4 Mo2 P4 162.27(3) . . ?
Cl4 Mo2 P3 90.45(3) . . ?
O2 Mo2 Cl5 164.81(8) . . ?
O2 Mo2 Cl6 100.94(8) . . ?
O2 Mo2 P4 90.46(8) . . ?
O2 Mo2 Cl4 102.88(8) . . ?
O2 Mo2 P3 87.23(8) . . ?
Cl3 Mo1 P2 80.34(3) . . ?
Cl3 Mo1 P1 76.00(3) . . ?
P2 Mo1 P1 78.84(2) . . ?
Cl1 Mo1 Cl3 89.19(3) . . ?
Cl1 Mo1 P2 168.36(3) . . ?
Cl1 Mo1 P1 93.77(3) . . ?
Cl1 Mo1 Cl2 96.98(3) . . ?
Cl2 Mo1 Cl3 88.76(3) . . ?
Cl2 Mo1 P2 87.93(3) . . ?
Cl2 Mo1 P1 161.21(3) . . ?
O1 Mo1 Cl3 162.42(8) . . ?
O1 Mo1 P2 88.71(8) . . ?
O1 Mo1 Cl1 100.17(8) . . ?
O1 Mo1 P1 88.47(8) . . ?
O1 Mo1 Cl2 104.66(8) . . ?
C00F P4 Mo2 111.48(11) . . ?
C00F P4 C00H 104.72(14) . . ?
C00F P4 C00M 105.98(14) . . ?
C00H P4 Mo2 108.94(10) . . ?
C00M P4 Mo2 117.77(10) . . ?
C00M P4 C00H 107.10(14) . . ?
C00I P2 Mo1 109.38(10) . . ?
C00K P2 Mo1 110.91(11) . . ?
C00K P2 C00I 106.15(14) . . ?
C00K P2 C00O 105.99(16) . . ?
C00O P2 Mo1 116.79(12) . . ?
C00O P2 C00I 107.04(15) . . ?
C00G P3 Mo2 109.56(10) . . ?
C00L P3 Mo2 116.77(11) . . ?
C00L P3 C00G 106.84(15) . . ?
C00L P3 C00Q 106.71(15) . . ?
C00Q P3 Mo2 111.91(12) . . ?
C00Q P3 C00G 104.19(15) . . ?
C00J P1 Mo1 108.18(10) . . ?
C00N P1 Mo1 115.40(12) . . ?
C00N P1 C00J 108.38(15) . . ?
C00N P1 C00P 104.42(17) . . ?
C00P P1 Mo1 114.50(12) . . ?
C00P P1 C00J 105.39(16) . . ?
C00H C00G P3 111.6(2) . . ?
C00G C00H P4 110.5(2) . . ?
C00J C00I P2 110.9(2) . . ?
C00I C00J P1 109.68(19) . . ?
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
Mo2 Cl5 2.5213(7) . ?
Mo2 Cl6 2.3655(7) . ?
Mo2 P4 2.5226(7) . ?
Mo2 Cl4 2.3942(7) . ?
Mo2 P3 2.5400(8) . ?
Mo2 O2 1.685(2) . ?
Mo1 Cl3 2.5011(7) . ?
Mo1 P2 2.5249(8) . ?
Mo1 Cl1 2.3825(8) . ?
Mo1 P1 2.5261(8) . ?
Mo1 Cl2 2.3835(8) . ?
Mo1 O1 1.680(2) . ?
P4 C00F 1.802(3) . ?
P4 C00H 1.823(3) . ?
P4 C00M 1.808(3) . ?
P2 C00I 1.836(3) . ?
P2 C00K 1.809(3) . ?
P2 C00O 1.809(3) . ?
P3 C00G 1.839(3) . ?
P3 C00L 1.800(3) . ?
P3 C00Q 1.807(3) . ?
P1 C00J 1.833(3) . ?
P1 C00N 1.804(3) . ?
P1 C00P 1.809(3) . ?
C00G C00H 1.528(4) . ?
C00I C00J 1.538(4) . ?
