#------------------------------------------------------------------------------
#$Date: 2017-04-28 04:34:23 +0200 (Fri 28 de Apr de 2017) $
#$Revision: 195838 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/28/7042827.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_7042827
loop_
_publ_author_name
'Solís-Huitrón, Josué'
'Zúñiga-Villarreal, Noé'
'Martínez-Otero, Diego'
'Barquera-Lozada, Jose Enrique'
_publ_section_title
;
 Delocalized and Localized Donating- Accepting Mn-C Interactions in
 Half-Sandwich Cyclopentadienyl and Pentadienyl Complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00499K
_journal_year                    2017
_chemical_formula_moiety         'C44 H42 Mn2 O4 P2'
_chemical_formula_sum            'C44 H42 Mn2 O4 P2'
_chemical_formula_weight         806.59
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-12-13 deposited with the CCDC.
2017-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                105.9466(6)
_cell_angle_beta                 112.2887(6)
_cell_angle_gamma                104.5166(7)
_cell_formula_units_Z            1
_cell_length_a                   9.5676(4)
_cell_length_b                   10.9197(4)
_cell_length_c                   11.2228(4)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.39
_cell_volume                     956.58(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_unetI/netI     0.0071
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30153
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.115
_diffrn_source                   'Incoatec ImuS'
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1, Sheldrick'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       Prism
_exptl_crystal_F_000             418
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0241
_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)+(0.0357P)²+0.6505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3586
_reflns_number_total             3641
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00499k2.cif
_cod_data_source_block           mo_135zvn14_0m
_cod_database_code               7042827
_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   0.761
_shelx_estimated_absorpt_t_max   0.912
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mn1 Mn 0.86352(2) 0.80166(2) 0.61604(2) 0.01397(8) Uani 1 1 d . .
P1 P 0.98540(4) 0.80469(3) 0.82931(3) 0.01073(9) Uani 1 1 d . .
O1 O 1.16310(15) 0.92670(15) 0.59963(13) 0.0387(3) Uani 1 1 d . .
O2 O 0.90371(18) 1.09402(12) 0.72339(13) 0.0358(3) Uani 1 1 d . .
C1 C 1.19998(16) 0.82199(14) 0.91112(15) 0.0137(3) Uani 1 1 d . .
C2 C 1.30401(17) 0.89560(14) 1.05646(15) 0.0166(3) Uani 1 1 d . .
H2 H 1.2642 0.9385 1.1148 0.020 Uiso 1 1 calc R U
C3 C 1.46600(18) 0.90664(15) 1.11664(16) 0.0196(3) Uani 1 1 d . .
H3 H 1.5372 0.9590 1.2154 0.024 Uiso 1 1 calc R U
C4 C 1.52333(18) 0.84129(16) 1.03257(17) 0.0210(3) Uani 1 1 d . .
H4 H 1.6336 0.8483 1.0738 0.025 Uiso 1 1 calc R U
C5 C 1.41982(19) 0.76562(16) 0.88833(17) 0.0218(3) Uani 1 1 d . .
H5 H 1.4586 0.7191 0.8312 0.026 Uiso 1 1 calc R U
C6 C 1.25896(18) 0.75758(15) 0.82692(16) 0.0185(3) Uani 1 1 d . .
H6 H 1.1895 0.7082 0.7276 0.022 Uiso 1 1 calc R U
C7 C 0.88497(16) 0.66201(14) 0.86370(14) 0.0132(3) Uani 1 1 d . .
C8 C 0.78222(18) 0.67277(15) 0.92315(15) 0.0185(3) Uani 1 1 d . .
H8 H 0.7671 0.7568 0.9505 0.022 Uiso 1 1 calc R U
C9 C 0.70167(19) 0.56116(17) 0.94270(17) 0.0241(3) Uani 1 1 d . .
H9 H 0.6306 0.5688 0.9822 0.029 Uiso 1 1 calc R U
C10 C 0.72460(19) 0.43910(16) 0.90485(17) 0.0254(3) Uani 1 1 d . .
H10 H 0.6703 0.3634 0.9194 0.031 Uiso 1 1 calc R U
C11 C 0.82687(19) 0.42724(15) 0.84570(17) 0.0237(3) Uani 1 1 d . .
H11 H 0.8427 0.3434 0.8198 0.028 Uiso 1 1 calc R U
C12 C 0.90629(18) 0.53807(15) 0.82435(15) 0.0180(3) Uani 1 1 d . .
H12 H 0.9753 0.5293 0.7828 0.022 Uiso 1 1 calc R U
C13 C 0.81632(19) 0.58028(15) 0.51802(15) 0.0201(3) Uani 1 1 d . .
H13A H 0.9140 0.5572 0.5356 0.024 Uiso 1 1 calc R U
H13B H 0.7263 0.5126 0.5190 0.024 Uiso 1 1 calc R U
C14 C 0.76969(19) 0.63424(15) 0.41551(15) 0.0205(3) Uani 1 1 d . .
C15 C 0.66374(19) 0.70615(15) 0.40476(15) 0.0216(3) Uani 1 1 d . .
H15 H 0.6660 0.7622 0.3480 0.026 Uiso 1 1 calc R U
C16 C 0.60257(18) 0.74545(16) 0.50047(16) 0.0227(3) Uani 1 1 d . .
C17 C 0.63006(18) 0.70840(17) 0.61501(16) 0.0222(3) Uani 1 1 d . .
H17A H 0.5896 0.6078 0.5925 0.027 Uiso 1 1 calc R U
H17B H 0.6138 0.7638 0.6909 0.027 Uiso 1 1 calc R U
C18 C 0.8482(2) 0.63078(18) 0.32114(17) 0.0294(4) Uani 1 1 d . .
H18A H 0.7811 0.5452 0.2343 0.044 Uiso 1 1 calc R U
H18B H 0.9590 0.6337 0.3706 0.044 Uiso 1 1 calc R U
H18C H 0.8553 0.7112 0.2973 0.044 Uiso 1 1 calc R U
C19 C 0.5222(2) 0.8474(2) 0.48607(19) 0.0365(4) Uani 1 1 d . .
H19A H 0.4027 0.7965 0.4264 0.055 Uiso 1 1 calc R U
H19B H 0.5653 0.9028 0.4427 0.055 Uiso 1 1 calc R U
H19C H 0.5465 0.9091 0.5798 0.055 Uiso 1 1 calc R U
C20 C 1.04682(19) 0.87347(17) 0.60586(15) 0.0233(3) Uani 1 1 d . .
C21 C 0.8854(2) 0.97894(16) 0.68179(16) 0.0230(3) Uani 1 1 d . .
C22 C 0.99884(16) 0.94902(14) 0.96090(14) 0.0130(3) Uani 1 1 d . .
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'
Mn Mn 0.3368 0.7283 '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
C20 Mn1 C21 84.16(7) .
C20 Mn1 C15 106.56(6) .
C21 Mn1 C15 104.94(6) .
C20 Mn1 C14 88.29(6) .
C21 Mn1 C14 137.88(6) .
C15 Mn1 C14 38.75(6) .
C20 Mn1 C16 139.56(6) .
C21 Mn1 C16 87.15(7) .
C15 Mn1 C16 38.80(6) .
C14 Mn1 C16 72.38(6) .
C20 Mn1 C17 176.66(6) .
C21 Mn1 C17 96.82(7) .
C15 Mn1 C17 70.10(6) .
C14 Mn1 C17 88.86(6) .
C16 Mn1 C17 37.54(6) .
C20 Mn1 C13 97.80(7) .
C21 Mn1 C13 174.78(6) .
C15 Mn1 C13 69.88(6) .
C14 Mn1 C13 37.74(6) .
C16 Mn1 C13 88.25(6) .
C17 Mn1 C13 80.95(6) .
C20 Mn1 P1 97.26(5) .
C21 Mn1 P1 94.17(5) .
C15 Mn1 P1 150.63(4) .
C14 Mn1 P1 127.91(4) .
C16 Mn1 P1 122.77(4) .
C17 Mn1 P1 85.86(4) .
C13 Mn1 P1 90.39(4) .
C22 P1 C7 100.52(6) .
C22 P1 C1 100.03(6) .
C7 P1 C1 101.28(6) .
C22 P1 Mn1 111.69(4) .
C7 P1 Mn1 118.49(4) .
C1 P1 Mn1 121.44(5) .
C6 C1 C2 119.31(13) .
C6 C1 P1 119.45(11) .
C2 C1 P1 121.23(10) .
C3 C2 C1 120.36(13) .
C4 C3 C2 120.02(14) .
C3 C4 C5 120.02(13) .
C4 C5 C6 120.18(14) .
C1 C6 C5 120.07(14) .
C8 C7 C12 119.20(13) .
C8 C7 P1 121.25(10) .
C12 C7 P1 119.50(10) .
C9 C8 C7 120.31(14) .
C10 C9 C8 120.23(14) .
C9 C10 C11 119.97(14) .
C10 C11 C12 120.05(14) .
C11 C12 C7 120.23(14) .
C14 C13 Mn1 68.69(8) .
C13 C14 C15 123.22(14) .
C13 C14 C18 119.69(14) .
C15 C14 C18 116.76(14) .
C13 C14 Mn1 73.57(8) .
C15 C14 Mn1 70.36(8) .
C18 C14 Mn1 124.60(11) .
C14 C15 C16 126.15(14) .
C14 C15 Mn1 70.89(8) .
C16 C15 Mn1 71.16(8) .
C17 C16 C15 123.79(14) .
C17 C16 C19 119.08(14) .
C15 C16 C19 116.67(15) .
C17 C16 Mn1 73.27(9) .
C15 C16 Mn1 70.04(8) .
C19 C16 Mn1 124.88(12) .
C16 C17 Mn1 69.19(9) .
O1 C20 Mn1 175.95(15) .
O2 C21 Mn1 177.82(15) .
C22 C22 P1 173.28(17) 2_777
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 C20 1.7931(16) .
Mn1 C21 1.7975(16) .
Mn1 C15 2.1372(15) .
Mn1 C14 2.1440(14) .
Mn1 C16 2.1518(15) .
Mn1 C17 2.2046(15) .
Mn1 C13 2.2074(14) .
Mn1 P1 2.2158(4) .
P1 C22 1.7767(14) .
P1 C7 1.8332(14) .
P1 C1 1.8368(14) .
O1 C20 1.157(2) .
O2 C21 1.154(2) .
C1 C6 1.394(2) .
C1 C2 1.394(2) .
C2 C3 1.393(2) .
C3 C4 1.385(2) .
C4 C5 1.387(2) .
C5 C6 1.395(2) .
C7 C8 1.392(2) .
C7 C12 1.3953(19) .
C8 C9 1.390(2) .
C9 C10 1.383(2) .
C10 C11 1.387(2) .
C11 C12 1.391(2) .
C13 C14 1.409(2) .
C14 C15 1.420(2) .
C14 C18 1.511(2) .
C15 C16 1.425(2) .
C16 C17 1.403(2) .
C16 C19 1.514(2) .
C22 C22 1.203(3) 2_777
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
C22 P1 C1 C6 -159.89(11)
C7 P1 C1 C6 97.14(12)
Mn1 P1 C1 C6 -36.66(13)
C22 P1 C1 C2 21.66(12)
C7 P1 C1 C2 -81.31(12)
Mn1 P1 C1 C2 144.90(10)
C6 C1 C2 C3 1.1(2)
P1 C1 C2 C3 179.50(11)
C1 C2 C3 C4 -1.7(2)
C2 C3 C4 C5 0.4(2)
C3 C4 C5 C6 1.4(2)
C2 C1 C6 C5 0.8(2)
P1 C1 C6 C5 -177.68(11)
C4 C5 C6 C1 -2.0(2)
C22 P1 C7 C8 27.48(13)
C1 P1 C7 C8 130.05(12)
Mn1 P1 C7 C8 -94.43(11)
C22 P1 C7 C12 -155.18(11)
C1 P1 C7 C12 -52.61(12)
Mn1 P1 C7 C12 82.91(11)
C12 C7 C8 C9 -0.1(2)
P1 C7 C8 C9 177.21(11)
C7 C8 C9 C10 0.8(2)
C8 C9 C10 C11 -0.7(2)
C9 C10 C11 C12 0.0(2)
C10 C11 C12 C7 0.7(2)
C8 C7 C12 C11 -0.6(2)
P1 C7 C12 C11 -178.01(11)
Mn1 C13 C14 C15 -52.27(13)
Mn1 C13 C14 C18 120.88(14)
C13 C14 C15 C16 6.2(2)
C18 C14 C15 C16 -167.12(15)
Mn1 C14 C15 C16 -47.43(15)
C13 C14 C15 Mn1 53.65(13)
C18 C14 C15 Mn1 -119.69(13)
C14 C15 C16 C17 -5.0(3)
Mn1 C15 C16 C17 -52.30(14)
C14 C15 C16 C19 167.22(16)
Mn1 C15 C16 C19 119.89(14)
C14 C15 C16 Mn1 47.33(14)
C15 C16 C17 Mn1 50.95(14)
C19 C16 C17 Mn1 -121.07(15)
