#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/50/2005034.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2005034
loop_
_publ_author_name
'bin Shawkataly, O.'
'Saminathan, T.'
'Muniswaran, K.'
'Fun, H.-K.'
'Sivakumar, K.'
_publ_section_title
;
 Pentacarbonyl[tris(2-methoxyphenyl)phosphine-P]chromium and its
 Molybdenum Analogue
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1352
_journal_page_last               1355
_journal_paper_doi               10.1107/S0108270196001527
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Mo (C21 H21 O3 P1) (C1 O1)5]'
_chemical_formula_sum            'C26 H21 Mo O8 P'
_chemical_formula_weight         588.34
_chemical_name_systematic
;
Pentacarbonyl tris(2-methoxyphenyl)phosphine Molybdenum(0).
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 92.570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.889(2)
_cell_length_b                   16.395(2)
_cell_length_c                   14.808(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      8
_cell_volume                     2640.9(7)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material
'SHELXL93; geometrical calculations: PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       θ/2θ
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7456
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.899
_refine_ls_goodness_of_fit_obs   1.020
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_restrained_S_obs      1.020
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_obs          0.0350
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0389P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0849
_refine_ls_wR_factor_obs         0.0781
_reflns_number_observed          4100
_reflns_number_total             6039
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1238.cif
_cod_data_source_block           comp2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2005034
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_occupancy
_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_calc_flag
_atom_site_type_symbol
Mo 1 .21639(2) .612015(14) .915027(15) .04504(8) Uani d Mo
P 1 .26133(6) .76401(4) .95028(4) .04017(15) Uani d P
O1 1 .2002(3) .6514(2) .7066(2) .0941(8) Uani d O
O2 1 .4936(2) .5629(2) .8857(2) .0950(9) Uani d O
O3 1 .2506(3) .5740(2) 1.1256(2) .1013(9) Uani d O
O4 1 -.0723(2) .6250(2) .9364(2) .0907(8) Uani d O
O5 1 .1587(3) .43066(14) .8642(2) .0981(9) Uani d O
O6 1 .2615(3) .94607(13) .9620(2) .0817(7) Uani d O
O7 1 .0574(2) .75695(13) 1.06777(13) .0602(5) Uani d O
O8 1 .4983(2) .70371(13) 1.01961(14) .0605(5) Uani d O
C1 1 .2035(3) .6381(2) .7820(2) .0589(7) Uani d C
C2 1 .3961(3) .5841(2) .8977(2) .0624(8) Uani d C
C3 1 .2382(3) .5871(2) 1.0508(2) .0614(8) Uani d C
C4 1 .0319(3) .6247(2) .9294(2) .0591(8) Uani d C
C5 1 .1798(3) .4967(2) .8842(2) .0640(8) Uani d C
C6 1 .1563(2) .8371(2) .8932(2) .0476(6) Uani d C
C7 1 .0611(3) .8096(2) .8351(2) .0545(7) Uani d C
C8 1 -.0229(3) .8618(3) .7928(2) .0712(9) Uani d C
C9 1 -.0139(4) .9434(3) .8110(3) .0850(12) Uani d C
C10 1 .0775(5) .9728(2) .8680(3) .0874(13) Uani d C
C11 1 .1641(3) .9208(2) .9084(2) .0639(8) Uani d C
C12 1 .2654(8) 1.0282(3) .9925(5) .115(2) Uani d C
C13 1 .2615(2) .8006(2) 1.0677(2) .0426(6) Uani d C
C14 1 .3614(3) .8387(2) 1.1109(2) .0537(7) Uani d C
C15 1 .3518(3) .8711(2) 1.1975(2) .0629(8) Uani d C
C16 1 .2445(3) .8661(2) 1.2399(2) .0680(9) Uani d C
C17 1 .1446(3) .8282(2) 1.1990(2) .0604(8) Uani d C
C18 1 .1523(3) .7953(2) 1.1132(2) .0477(6) Uani d C
C19 1 -.0619(3) .7648(3) 1.1005(4) .0795(11) Uani d C
C20 1 .4123(2) .7930(2) .9116(2) .0470(6) Uani d C
C21 1 .4253(3) .8458(2) .8400(2) .0615(8) Uani d C
C22 1 .5404(4) .8642(3) .8085(3) .0809(11) Uani d C
C23 1 .6407(4) .8292(3) .8478(3) .0891(15) Uani d C
C24 1 .6329(3) .7747(3) .9192(3) .0734(10) Uani d C
C25 1 .5179(3) .7565(2) .9515(2) .0542(7) Uani d C
C26 1 .6015(4) .6647(3) 1.0632(3) .0822(12) Uani d C
H6 1 -.092(3) .8413(19) .7470(18) .064(9) Uiso d H
H7 1 .058(3) .749(2) .825(2) .074(10) Uiso d H
H9 1 -.073(4) .982(3) .781(3) .121(15) Uiso d H
H10 1 .087(3) 1.024(2) .877(2) .077(11) Uiso d H
H12A 1 .350(4) 1.026(3) 1.027(3) .107(15) Uiso d H
H12B 1 .306(5) 1.047(3) .944(3) .12(2) Uiso d H
H12C 1 .191(6) 1.047(4) 1.025(4) .19(3) Uiso d H
H14 1 .428(2) .8493(16) 1.0803(16) .040(7) Uiso d H
H15 1 .413(3) .8971(18) 1.2209(19) .054(8) Uiso d H
H16 1 .240(3) .8846(18) 1.302(2) .067(9) Uiso d H
H17 1 .077(3) .8225(18) 1.2251(18) .051(8) Uiso d H
H19A 1 -0.112(4) .741(2) 1.054(3) .091(13) Uiso d H
H19B 1 -.078(4) .824(3) 1.082(3) .122(16) Uiso d H
H19C 1 -.061(6) .755(4) 1.159(4) .19(3) Uiso d H
H21 1 .357(3) .8719(17) .8130(18) .049(8) Uiso d H
H22 1 .550(4) .898(2) .763(3) .095(14) Uiso d H
H23 1 .709(3) .838(2) .832(2) .074(11) Uiso d H
H24 1 .702(3) .751(2) .949(2) .075(10) Uiso d H
H26A 1 .652(4) .635(3) 1.023(3) .100(14) Uiso d H
H26B 1 .571(4) .631(3) 1.109(3) .093(14) Uiso d H
H26C 1 .651(4) .706(3) 1.098(3) .124(16) Uiso d H
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'
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'
Mo Mo -1.6832 0.6857 '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
C5 Mo C1 88.44(13)
C5 Mo C2 86.63(14)
C1 Mo C2 87.10(13)
C5 Mo C4 86.14(13)
C1 Mo C4 93.13(12)
C2 Mo C4 172.76(13)
C5 Mo C3 92.81(13)
C1 Mo C3 177.27(13)
C2 Mo C3 90.55(13)
C4 Mo C3 89.38(12)
C5 Mo P 178.19(9)
C1 Mo P 89.85(9)
C2 Mo P 93.88(9)
C4 Mo P 93.36(9)
C3 Mo P 88.92(9)
C20 P C6 103.68(13)
C20 P C13 104.39(12)
C6 P C13 101.37(12)
C20 P Mo 110.59(9)
C6 P Mo 115.29(9)
C13 P Mo 119.78(9)
C11 O6 C12 119.1(4)
C18 O7 C19 118.6(3)
C25 O8 C26 118.5(3)
O1 C1 Mo 177.5(3)
O2 C2 Mo 174.8(3)
O3 C3 Mo 179.5(3)
O4 C4 Mo 174.3(3)
O5 C5 Mo 178.3(3)
C11 C6 C7 117.3(3)
C11 C6 P 122.4(2)
C7 C6 P 120.3(2)
C8 C7 C6 122.6(3)
C9 C8 C7 118.5(4)
C10 C9 C8 120.8(4)
C9 C10 C11 120.8(4)
O6 C11 C10 124.1(3)
O6 C11 C6 115.8(3)
C10 C11 C6 120.0(3)
C14 C13 C18 118.3(2)
C14 C13 P 123.5(2)
C18 C13 P 118.1(2)
C13 C14 C15 120.4(3)
C16 C15 C14 120.3(3)
C15 C16 C17 120.5(3)
C16 C17 C18 120.1(3)
O7 C18 C17 123.8(3)
O7 C18 C13 115.8(2)
C17 C18 C13 120.4(3)
C21 C20 C25 118.7(3)
C21 C20 P 121.9(2)
C25 C20 P 119.3(2)
C20 C21 C22 121.3(4)
C23 C22 C21 119.3(4)
C22 C23 C24 121.8(4)
C23 C24 C25 119.1(4)
O8 C25 C24 124.6(3)
O8 C25 C20 115.6(2)
C24 C25 C20 119.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo C5 1.981(3)
Mo C1 2.015(3)
Mo C2 2.037(4)
Mo C4 2.040(3)
Mo C3 2.055(3)
Mo P 2.5883(7)
P C20 1.828(3)
P C6 1.837(3)
P C13 1.839(3)
O1 C1 1.137(3)
O2 C2 1.139(4)
O3 C3 1.131(4)
O4 C4 1.144(4)
O5 C5 1.143(4)
O6 C11 1.361(4)
O6 C12 1.420(5)
O7 C18 1.361(3)
O7 C19 1.412(4)
O8 C25 1.354(4)
O8 C26 1.423(4)
C6 C11 1.392(4)
C6 C7 1.392(4)
C7 C8 1.381(4)
C8 C9 1.368(6)
C9 C10 1.363(6)
C10 C11 1.388(5)
C13 C14 1.386(4)
C13 C18 1.396(4)
C14 C15 1.396(4)
C15 C16 1.353(5)
C16 C17 1.370(5)
C17 C18 1.388(4)
C20 C21 1.381(4)
C20 C25 1.403(4)
C21 C22 1.389(5)
C22 C23 1.344(6)
C23 C24 1.389(6)
C24 C25 1.392(4)
