#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:22:05 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178622 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/33/4073340.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_4073340
loop_
_publ_author_name
'Buccella, Daniela'
'Tanski, Joseph M.'
'Parkin, Gerard'
_publ_section_title
;
 Factors Influencing Coordination versus Oxidative Addition of C−H
 Bonds to Molybdenum and Tungsten:  Structural and Spectroscopic
 Evidence That the Calixarene Framework Promotes C−H Bond
 Activation
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3275
_journal_paper_doi               10.1021/om700279c
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C26 H47 Mo O2 P3'
_chemical_formula_weight         580.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.757(2)
_cell_angle_beta                 76.411(2)
_cell_angle_gamma                80.895(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8431(10)
_cell_length_b                   11.2629(13)
_cell_length_c                   15.8528(18)
_cell_measurement_reflns_used    6936
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      26.242
_cell_measurement_theta_min      2.413
_cell_volume                     1502.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10109
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.9134
_exptl_absorpt_correction_T_min  0.8868
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0650P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0905
_reflns_number_gt                5783
_reflns_number_total             6518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700279c-file004.cif
_cod_data_source_block           phmos10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073340
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Mo Mo 0.203189(19) 0.224110(15) 0.230393(10) 0.02767(7) Uani 1 1 d .
H1 H 0.301(3) 0.114(2) 0.1730(16) 0.043(7) Uiso 1 1 d .
H2 H 0.096(3) 0.138(2) 0.1996(15) 0.041(6) Uiso 1 1 d .
P1 P 0.48279(7) 0.21279(5) 0.20130(4) 0.03921(14) Uani 1 1 d .
P2 P 0.17443(7) 0.02535(5) 0.31656(4) 0.03699(14) Uani 1 1 d .
P3 P 0.18622(7) 0.26364(5) 0.07702(4) 0.03619(13) Uani 1 1 d .
O1 O 0.20873(18) 0.25894(14) 0.35520(10) 0.0376(3) Uani 1 1 d .
O2 O 0.19696(17) 0.41479(13) 0.20247(10) 0.0359(3) Uani 1 1 d .
C1 C -0.0993(3) 0.3453(2) 0.31104(14) 0.0332(4) Uani 1 1 d .
H3 H -0.031(3) 0.276(2) 0.2720(16) 0.044(7) Uiso 1 1 d .
H4 H -0.210(3) 0.335(2) 0.3171(15) 0.034(6) Uiso 1 1 d .
C10 C 0.0873(3) 0.30069(18) 0.41576(13) 0.0330(4) Uani 1 1 d .
C11 C -0.0642(3) 0.33519(19) 0.40088(13) 0.0337(4) Uani 1 1 d .
C12 C -0.1867(3) 0.3724(2) 0.46860(15) 0.0397(5) Uani 1 1 d .
H12A H -0.2886 0.3924 0.4582 0.048 Uiso 1 1 calc R
C13 C -0.1624(3) 0.3807(2) 0.55064(14) 0.0423(5) Uani 1 1 d .
C14 C -0.0114(3) 0.3479(2) 0.56456(14) 0.0428(5) Uani 1 1 d .
H14A H 0.0074 0.3531 0.6197 0.051 Uiso 1 1 calc R
C15 C 0.1130(3) 0.3076(2) 0.49974(14) 0.0387(5) Uani 1 1 d .
C16 C 0.2747(3) 0.2733(3) 0.51770(17) 0.0538(7) Uani 1 1 d .
H16A H 0.2721 0.2836 0.5776 0.081 Uiso 1 1 calc R
H16B H 0.3458 0.3250 0.4781 0.081 Uiso 1 1 calc R
H16C H 0.3105 0.1894 0.5090 0.081 Uiso 1 1 calc R
C17 C -0.2949(4) 0.4274(3) 0.62175(17) 0.0585(7) Uani 1 1 d .
H17A H -0.3912 0.4453 0.6004 0.088 Uiso 1 1 calc R
H17B H -0.2703 0.5005 0.6378 0.088 Uiso 1 1 calc R
H17C H -0.3078 0.3661 0.6726 0.088 Uiso 1 1 calc R
C20 C 0.0709(2) 0.49732(18) 0.21310(13) 0.0306(4) Uani 1 1 d .
C21 C 0.0860(3) 0.61870(19) 0.17564(13) 0.0348(5) Uani 1 1 d .
C22 C -0.0457(3) 0.7051(2) 0.18431(14) 0.0397(5) Uani 1 1 d .
H22A H -0.0340 0.7856 0.1594 0.048 Uiso 1 1 calc R
C23 C -0.1938(3) 0.6775(2) 0.22825(15) 0.0422(5) Uani 1 1 d .
C24 C -0.2069(3) 0.5584(2) 0.26509(14) 0.0372(5) Uani 1 1 d .
H24A H -0.3061 0.5374 0.2948 0.045 Uiso 1 1 calc R
C25 C -0.0785(2) 0.46888(19) 0.25968(13) 0.0320(4) Uani 1 1 d .
C26 C 0.2448(3) 0.6521(2) 0.12672(16) 0.0445(5) Uani 1 1 d .
H26A H 0.2360 0.7382 0.1057 0.067 Uiso 1 1 calc R
H26B H 0.2828 0.6064 0.0774 0.067 Uiso 1 1 calc R
H26C H 0.3176 0.6333 0.1656 0.067 Uiso 1 1 calc R
C27 C -0.3354(3) 0.7731(3) 0.23677(19) 0.0616(8) Uani 1 1 d .
H27A H -0.4276 0.7362 0.2690 0.092 Uiso 1 1 calc R
H27B H -0.3507 0.8085 0.1790 0.092 Uiso 1 1 calc R
H27C H -0.3189 0.8358 0.2678 0.092 Uiso 1 1 calc R
C31 C 0.5785(4) 0.1458(3) 0.2908(2) 0.0715(9) Uani 1 1 d .
H31A H 0.6909 0.1462 0.2713 0.107 Uiso 1 1 calc R
H31B H 0.5556 0.0630 0.3093 0.107 Uiso 1 1 calc R
H31C H 0.5399 0.1926 0.3396 0.107 Uiso 1 1 calc R
C32 C 0.6047(3) 0.1351(3) 0.1121(2) 0.0685(9) Uani 1 1 d .
H32A H 0.7143 0.1395 0.1098 0.103 Uiso 1 1 calc R
H32B H 0.5784 0.1735 0.0572 0.103 Uiso 1 1 calc R
H32C H 0.5864 0.0508 0.1216 0.103 Uiso 1 1 calc R
C33 C 0.5468(3) 0.3626(2) 0.1780(2) 0.0592(8) Uani 1 1 d .
H33A H 0.6604 0.3545 0.1665 0.089 Uiso 1 1 calc R
H33B H 0.5033 0.4064 0.2279 0.089 Uiso 1 1 calc R
H33C H 0.5108 0.4067 0.1271 0.089 Uiso 1 1 calc R
C41 C -0.0243(3) 0.0155(3) 0.3786(2) 0.0635(8) Uani 1 1 d .
H41A H -0.0307 -0.0644 0.4117 0.095 Uiso 1 1 calc R
H41B H -0.0954 0.0294 0.3387 0.095 Uiso 1 1 calc R
H41C H -0.0533 0.0763 0.4184 0.095 Uiso 1 1 calc R
C42 C 0.2882(4) -0.0337(3) 0.4000(2) 0.0644(8) Uani 1 1 d .
H42A H 0.2608 -0.1132 0.4270 0.097 Uiso 1 1 calc R
H42B H 0.2651 0.0208 0.4442 0.097 Uiso 1 1 calc R
H42C H 0.3992 -0.0400 0.3731 0.097 Uiso 1 1 calc R
C43 C 0.2083(4) -0.1046(2) 0.2573(2) 0.0633(8) Uani 1 1 d .
H43A H 0.1937 -0.1776 0.2985 0.095 Uiso 1 1 calc R
H43B H 0.3145 -0.1115 0.2225 0.095 Uiso 1 1 calc R
H43C H 0.1346 -0.0944 0.2192 0.095 Uiso 1 1 calc R
C51 C -0.0062(3) 0.3340(3) 0.06013(17) 0.0555(7) Uani 1 1 d .
H51A H -0.0051 0.3473 -0.0020 0.083 Uiso 1 1 calc R
H51B H -0.0318 0.4110 0.0834 0.083 Uiso 1 1 calc R
H51C H -0.0842 0.2811 0.0900 0.083 Uiso 1 1 calc R
C52 C 0.3089(4) 0.3653(3) -0.00032(17) 0.0597(7) Uani 1 1 d .
H52A H 0.2866 0.3701 -0.0579 0.090 Uiso 1 1 calc R
H52B H 0.4184 0.3346 -0.0026 0.090 Uiso 1 1 calc R
H52C H 0.2870 0.4453 0.0183 0.090 Uiso 1 1 calc R
C53 C 0.2165(4) 0.1338(3) 0.01717(18) 0.0647(8) Uani 1 1 d .
H53A H 0.2068 0.1615 -0.0427 0.097 Uiso 1 1 calc R
H53B H 0.1384 0.0800 0.0449 0.097 Uiso 1 1 calc R
H53C H 0.3204 0.0906 0.0175 0.097 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
H2 Mo H1 63.4(11)
H2 Mo H3 68.4(11)
H1 Mo H3 131.9(11)
H2 Mo O1 130.4(8)
H1 Mo O1 130.6(8)
H3 Mo O1 82.1(7)
H2 Mo O2 127.4(8)
H1 Mo O2 131.0(8)
H3 Mo O2 79.8(7)
O1 Mo O2 82.19(6)
H2 Mo P1 128.3(8)
H1 Mo P1 64.8(8)
H3 Mo P1 163.3(7)
O1 Mo P1 85.58(4)
O2 Mo P1 87.35(4)
H2 Mo P3 64.2(8)
H1 Mo P3 67.0(9)
H3 Mo P3 92.5(7)
O1 Mo P3 159.10(5)
O2 Mo P3 76.97(4)
P1 Mo P3 95.01(2)
H2 Mo P2 63.4(8)
H1 Mo P2 69.2(8)
H3 Mo P2 89.8(7)
O1 Mo P2 78.14(5)
O2 Mo P2 158.86(4)
P1 Mo P2 98.70(2)
P3 Mo P2 122.22(2)
H2 Mo C1 84.0(8)
H1 Mo C1 147.4(8)
H3 Mo C1 15.5(7)
O1 Mo C1 70.15(6)
O2 Mo C1 69.08(6)
P1 Mo C1 147.77(4)
P3 Mo C1 100.40(5)
P2 Mo C1 96.72(5)
C33 P1 C32 103.05(15)
C33 P1 C31 100.71(15)
C32 P1 C31 100.97(17)
C33 P1 Mo 111.71(9)
C32 P1 Mo 120.66(11)
C31 P1 Mo 117.04(11)
C41 P2 C43 101.27(15)
C41 P2 C42 101.68(15)
C43 P2 C42 99.97(15)
C41 P2 Mo 112.07(10)
C43 P2 Mo 117.40(10)
C42 P2 Mo 121.48(10)
C52 P3 C53 100.94(15)
C52 P3 C51 99.84(14)
C53 P3 C51 100.93(15)
C52 P3 Mo 120.77(10)
C53 P3 Mo 117.57(10)
C51 P3 Mo 113.57(9)
C10 O1 Mo 127.10(14)
C20 O2 Mo 127.19(13)
C25 C1 C11 112.15(17)
C25 C1 Mo 96.43(12)
C11 C1 Mo 95.69(13)
O1 C10 C11 123.26(19)
O1 C10 C15 118.4(2)
C11 C10 C15 118.37(19)
C10 C11 C12 120.0(2)
C10 C11 C1 122.21(18)
C12 C11 C1 117.5(2)
C13 C12 C11 122.0(2)
C14 C13 C12 117.6(2)
C14 C13 C17 121.1(2)
C12 C13 C17 121.2(2)
C13 C14 C15 122.3(2)
C14 C15 C10 119.7(2)
C14 C15 C16 120.4(2)
C10 C15 C16 119.9(2)
O2 C20 C25 122.82(19)
O2 C20 C21 118.91(18)
C25 C20 C21 118.27(18)
C22 C21 C20 119.4(2)
C22 C21 C26 121.1(2)
C20 C21 C26 119.43(19)
C23 C22 C21 122.7(2)
C24 C23 C22 117.2(2)
C24 C23 C27 120.9(2)
C22 C23 C27 121.8(2)
C23 C24 C25 122.4(2)
C24 C25 C20 119.9(2)
C24 C25 C1 118.84(19)
C20 C25 C1 121.01(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo H2 1.66(2)
Mo H1 1.66(2)
Mo H3 2.04(2)
Mo O1 2.0909(14)
Mo O2 2.1166(15)
Mo P1 2.3928(7)
Mo P3 2.4362(6)
Mo P2 2.4446(6)
Mo C1 2.907(2)
P1 C33 1.818(3)
P1 C32 1.820(3)
P1 C31 1.821(3)
P2 C41 1.812(3)
P2 C43 1.813(3)
P2 C42 1.827(3)
P3 C52 1.819(3)
P3 C53 1.820(3)
P3 C51 1.821(3)
O1 C10 1.340(2)
O2 C20 1.330(2)
C1 C25 1.510(3)
C1 C11 1.511(3)
C10 C11 1.399(3)
C10 C15 1.418(3)
C11 C12 1.399(3)
C12 C13 1.387(3)
C13 C14 1.387(4)
C13 C17 1.515(3)
C14 C15 1.391(3)
C15 C16 1.501(4)
C20 C25 1.412(3)
C20 C21 1.414(3)
C21 C22 1.390(3)
C21 C26 1.508(3)
C22 C23 1.388(4)
C23 C24 1.386(3)
C23 C27 1.512(3)
C24 C25 1.390(3)
