#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:41:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178911 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/40/4114033.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_4114033
loop_
_publ_author_name
'Frances H. Stephens'
'Joshua S. Figueroa'
'Paula L. Diaconescu'
'Christopher C. Cummins'
_publ_section_title
;
 Molybdenum-Phosphorus Triple Bond Stabilization by Ancillary Alkoxide
 Ligation: Synthesis and Structure of a Terminal Phosphide
 Tris-1-methylcyclohexanoxide Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9264
_journal_page_last               9265
_journal_paper_doi               10.1021/ja0354317
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C21 H39 Mo O3 P'
_chemical_formula_weight         466.43
_chemical_name_common            PMo(O(1-MeCy))3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   10.8130(4)
_cell_length_b                   10.8130(4)
_cell_length_c                   69.271(3)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    183(2)
_cell_volume                     7014.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD 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  0.0879
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       76
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            8573
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.646
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0586P)²+12.6036P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                1016
_reflns_number_total             1127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0354317si20030616_025104_1.cif
_cod_data_source_block           002174m
_cod_original_cell_volume        7014.2(5)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4114033
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Mo1 Mo 0.3333 0.6667 0.047083(6) 0.0262(2) Uani 1 3 d S
P1 P 0.3333 0.6667 0.07761(2) 0.0437(5) Uani 1 3 d S
O1 O 0.4495(2) 0.8536(2) 0.03889(3) 0.0292(5) Uani 1 1 d .
C11 C 0.5536(3) 0.9949(3) 0.04595(4) 0.0316(7) Uani 1 1 d .
C12 C 0.6027(4) 1.0905(4) 0.02827(5) 0.0390(8) Uani 1 1 d .
H12A H 0.526(4) 1.085(4) 0.0223(5) 0.045(10) Uiso 1 1 d .
H12B H 0.661(4) 1.178(4) 0.0322(4) 0.041(9) Uiso 1 1 d .
C13 C 0.6798(4) 1.0494(4) 0.01369(5) 0.0434(8) Uani 1 1 d .
H13A H 0.709(4) 1.116(4) 0.0032(5) 0.056(10) Uiso 1 1 d .
H13B H 0.619(4) 0.964(4) 0.0088(4) 0.036(8) Uiso 1 1 d .
C14 C 0.8045(4) 1.0440(4) 0.02293(5) 0.0476(9) Uani 1 1 d .
H14A H 0.847(3) 1.016(3) 0.0135(5) 0.045(9) Uiso 1 1 d .
H14B H 0.872(4) 1.128(4) 0.0268(6) 0.060(13) Uiso 1 1 d .
C15 C 0.7557(4) 0.9448(4) 0.04011(5) 0.0417(8) Uani 1 1 d .
H15A H 0.692(4) 0.847(4) 0.0351(5) 0.046(10) Uiso 1 1 d .
H15B H 0.836(4) 0.948(3) 0.0466(4) 0.037(8) Uiso 1 1 d .
C16 C 0.6779(3) 0.9855(4) 0.05476(4) 0.0356(7) Uani 1 1 d .
H16A H 0.647(3) 0.924(3) 0.0650(4) 0.038(9) Uiso 1 1 d .
H16B H 0.744(3) 1.080(3) 0.0602(4) 0.035(8) Uiso 1 1 d .
C17 C 0.4824(4) 1.0427(4) 0.06063(5) 0.0470(8) Uani 1 1 d .
H17D H 0.4049 1.0475 0.0546 0.070 Uiso 1 1 calc R
H17A H 0.5507 1.1352 0.0655 0.070 Uiso 1 1 calc R
H17B H 0.4462 0.9756 0.0711 0.070 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Mo1 O1 111.10(5) 2_665 .
O1 Mo1 O1 111.10(5) 2_665 3_565
O1 Mo1 O1 111.10(5) . 3_565
O1 Mo1 P1 107.79(6) 2_665 .
O1 Mo1 P1 107.79(6) . .
O1 Mo1 P1 107.79(6) 3_565 .
C11 O1 Mo1 141.92(16) . .
O1 C11 C17 108.9(2) . .
O1 C11 C12 105.5(2) . .
C17 C11 C12 111.9(3) . .
O1 C11 C16 108.0(2) . .
C17 C11 C16 111.7(3) . .
C12 C11 C16 110.4(3) . .
C13 C12 C11 113.3(3) . .
C12 C13 C14 111.2(3) . .
C15 C14 C13 110.9(3) . .
C14 C15 C16 111.6(3) . .
C15 C16 C11 112.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.857(2) 2_665
Mo1 O1 1.857(2) .
Mo1 O1 1.857(2) 3_565
Mo1 P1 2.1144(16) .
O1 C11 1.456(3) .
C11 C17 1.514(4) .
C11 C12 1.517(4) .
C11 C16 1.525(4) .
C12 C13 1.511(5) .
C13 C14 1.520(5) .
C14 C15 1.510(5) .
C15 C16 1.517(4) .
