#------------------------------------------------------------------------------
#$Date: 2015-12-09 15:20:38 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171103 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/61/7036159.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_7036159
loop_
_publ_author_name
'Gupta, Vijay'
'Khullar, Sadhika'
'Kumar, Sandeep'
'Mandal, Sanjay K.'
_publ_section_title
;
 Construction of a robust pillared-layer framework based on the rare
 paddlewheel subunit [Mn(μ-O2CR)4L2]: synthesis, crystal structure and
 magnetic properties.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16778
_journal_page_last               16784
_journal_paper_doi               10.1039/c5dt02354h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C42 H36 Mn2 N2 O8 Si2'
_chemical_formula_sum            'C42 H36 Mn2 N2 O8 Si2'
_chemical_formula_weight         862.79
_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_update_record
;
2015-08-07 deposited with the CCDC.
2015-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                73.176(3)
_cell_angle_beta                 81.737(3)
_cell_angle_gamma                86.247(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6185(17)
_cell_length_b                   10.683(2)
_cell_length_c                   11.709(2)
_cell_measurement_reflns_used    2189
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      21.1802
_cell_measurement_theta_min      2.3901
_cell_volume                     1020.9(3)
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS)'
_computing_publication_material  'SHELXTL (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.1464
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5838
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.607
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.0800P)²]
where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2009
_reflns_number_gt                2145
_reflns_number_total             3421
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02354h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7036159--7036160.cif.'
_cod_database_code               7036159
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Mn Mn1 0.62087(10) 0.56930(8) 0.53804(8) 0.0315(3) Uani d . 1
Si Si2 -0.2465(2) 0.75336(16) 0.99944(16) 0.0363(5) Uani d . 1
O O1 0.4229(5) 0.6124(4) 0.6518(4) 0.0502(12) Uani d . 1
O O2 0.5014(6) 0.6822(5) 0.3917(4) 0.0600(14) Uani d . 1
O O3 0.7542(5) 0.4886(4) 0.4094(4) 0.0476(12) Uani d . 1
O O4 0.6842(6) 0.4003(5) 0.6741(4) 0.0574(14) Uani d . 1
N N1 0.7711(6) 0.7271(5) 0.5269(5) 0.0421(13) Uani d . 1
C C1 -0.0840(7) 0.6953(6) 0.9006(6) 0.0377(15) Uani d . 1
C C2 0.2850(8) 0.5787(6) 0.6551(6) 0.0401(16) Uani d . 1
C C3 0.1579(7) 0.6168(6) 0.7416(6) 0.0359(15) Uani d . 1
C C4 0.0094(8) 0.5718(6) 0.7576(6) 0.0422(16) Uani d . 1
H H4 -0.0135 0.5159 0.7147 0.051 Uiso calc R 1
C C5 -0.1080(7) 0.6083(6) 0.8372(6) 0.0420(16) Uani d . 1
H H5 -0.2067 0.573 0.8484 0.05 Uiso calc R 1
C C6 0.0678(8) 0.7410(7) 0.8820(7) 0.056(2) Uani d . 1
H H6 0.0905 0.7994 0.9224 0.067 Uiso calc R 1
C C7 0.1864(8) 0.7019(7) 0.8052(7) 0.0522(19) Uani d . 1
H H7 0.2868 0.7334 0.7963 0.063 Uiso calc R 1
C C8 -0.1747(8) 0.7661(6) 1.1373(6) 0.0468(17) Uani d . 1
H H8A -0.1174 0.6874 1.172 0.07 Uiso calc R 1
H H8B -0.2622 0.7781 1.1941 0.07 Uiso calc R 1
H H8C -0.1071 0.8394 1.117 0.07 Uiso calc R 1
C C9 -0.4144(8) 0.6415(7) 1.0342(6) 0.0544(19) Uani d . 1
H H9A -0.446 0.636 0.9605 0.082 Uiso calc R 1
H H9B -0.5006 0.6748 1.0796 0.082 Uiso calc R 1
H H9C -0.3833 0.5561 1.0805 0.082 Uiso calc R 1
C C10 -0.3047(7) 0.9233(6) 0.9093(6) 0.0391(16) Uani d . 1
C C11 -0.4272(8) 0.9463(7) 0.8393(6) 0.0502(18) Uani d . 1
H H11 -0.4894 0.8773 0.842 0.06 Uiso calc R 1
C C12 -0.2187(8) 1.0307(6) 0.9032(6) 0.0489(18) Uani d . 1
H H12 -0.1372 1.0193 0.9497 0.059 Uiso calc R 1
C C13 0.6028(8) 0.3084(7) 0.6743(6) 0.0451(18) Uani d . 1
C C14 0.6316(7) 0.1746(6) 0.7576(5) 0.0367(15) Uani d . 1
C C15 0.5421(8) 0.0702(7) 0.7657(6) 0.0486(18) Uani d . 1
H H15 0.4588 0.0828 0.7208 0.058 Uiso calc R 1
C C16 0.7497(8) 0.1549(6) 0.8301(7) 0.0506(19) Uani d . 1
H H16 0.8082 0.2251 0.8298 0.061 Uiso calc R 1
C C17 0.9174(8) 0.7358(7) 0.4754(8) 0.063(2) Uani d . 1
H H17 0.9612 0.6679 0.4455 0.075 Uiso calc R 1
C C18 1.0088(8) 0.8409(8) 0.4638(8) 0.068(3) Uani d . 1
H H18 1.1119 0.842 0.4268 0.081 Uiso calc R 1
C C19 0.9511(8) 0.9425(7) 0.5052(7) 0.0487(18) Uani d . 1
C C20 0.8019(11) 0.9323(10) 0.5610(12) 0.135(6) Uani d . 1
H H20 0.7552 0.9988 0.5917 0.162 Uiso calc R 1
C C21 0.7193(10) 0.8209(9) 0.5718(11) 0.122(5) Uani d . 1
H H21 0.6191 0.8137 0.6146 0.147 Uiso calc R 1
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'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O3 Mn1 O1 . . 158.89(18)
O3 Mn1 O4 . . 88.06(18)
O1 Mn1 O4 . . 92.45(18)
O3 Mn1 O2 . . 85.59(18)
O1 Mn1 O2 . . 85.90(18)
O4 Mn1 O2 . . 157.4(2)
O3 Mn1 N1 . . 99.11(19)
O1 Mn1 N1 . . 100.65(19)
O4 Mn1 N1 . . 109.1(2)
O2 Mn1 N1 . . 93.3(2)
O3 Mn1 Mn1 . 2_666 77.22(13)
O1 Mn1 Mn1 . 2_666 81.69(13)
O4 Mn1 Mn1 . 2_666 94.06(15)
O2 Mn1 Mn1 . 2_666 63.37(15)
N1 Mn1 Mn1 . 2_666 156.49(15)
C8 Si2 C9 . . 112.2(3)
C8 Si2 C1 . . 110.4(3)
C9 Si2 C1 . . 109.4(3)
C8 Si2 C10 . . 108.3(3)
C9 Si2 C10 . . 110.6(3)
C1 Si2 C10 . . 105.8(3)
C2 O1 Mn1 . . 125.5(4)
C13 O2 Mn1 2_666 . 149.6(5)
C2 O3 Mn1 2_666 . 131.6(4)
C13 O4 Mn1 . . 108.2(5)
C21 N1 C17 . . 115.7(6)
C21 N1 Mn1 . . 120.4(5)
C17 N1 Mn1 . . 123.9(5)
C5 C1 C6 . . 115.4(6)
C5 C1 Si2 . . 122.5(5)
C6 C1 Si2 . . 122.1(5)
O1 C2 O3 . 2_666 123.9(6)
O1 C2 C3 . . 118.8(6)
O3 C2 C3 2_666 . 117.2(6)
C4 C3 C7 . . 117.8(6)
C4 C3 C2 . . 121.2(6)
C7 C3 C2 . . 121.0(6)
C3 C4 C5 . . 120.9(6)
C3 C4 H4 . . 119.6
C5 C4 H4 . . 119.6
C1 C5 C4 . . 122.8(6)
C1 C5 H5 . . 118.6
C4 C5 H5 . . 118.6
C7 C6 C1 . . 122.0(6)
C7 C6 H6 . . 119.0
C1 C6 H6 . . 119.0
C3 C7 C6 . . 121.2(6)
C3 C7 H7 . . 119.4
C6 C7 H7 . . 119.4
Si2 C8 H8A . . 109.5
Si2 C8 H8B . . 109.5
H8A C8 H8B . . 109.5
Si2 C8 H8C . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
Si2 C9 H9A . . 109.5
Si2 C9 H9B . . 109.5
H9A C9 H9B . . 109.5
Si2 C9 H9C . . 109.5
H9A C9 H9C . . 109.5
H9B C9 H9C . . 109.5
C12 C10 C11 . . 116.6(6)
C12 C10 Si2 . . 120.8(5)
C11 C10 Si2 . . 122.5(5)
C15 C11 C10 1_465 . 121.2(6)
C15 C11 H11 1_465 . 119.4
C10 C11 H11 . . 119.4
C10 C12 C16 . 1_465 122.2(6)
C10 C12 H12 . . 118.9
C16 C12 H12 1_465 . 118.9
O4 C13 O2 . 2_666 124.6(7)
O4 C13 C14 . . 118.9(7)
O2 C13 C14 2_666 . 116.5(7)
C15 C14 C16 . . 118.1(6)
C15 C14 C13 . . 121.9(6)
C16 C14 C13 . . 120.0(6)
C14 C15 C11 . 1_645 121.6(6)
C14 C15 H15 . . 119.2
C11 C15 H15 1_645 . 119.2
C14 C16 C12 . 1_645 120.3(6)
C14 C16 H16 . . 119.8
C12 C16 H16 1_645 . 119.8
N1 C17 C18 . . 122.9(6)
N1 C17 H17 . . 118.5
C18 C17 H17 . . 118.5
C19 C18 C17 . . 121.0(6)
C19 C18 H18 . . 119.5
C17 C18 H18 . . 119.5
C18 C19 C20 . . 116.1(7)
C18 C19 C19 . 2_776 122.0(7)
C20 C19 C19 . 2_776 121.8(8)
C19 C20 C21 . . 119.1(8)
C19 C20 H20 . . 120.5
C21 C20 H20 . . 120.5
N1 C21 C20 . . 124.9(7)
N1 C21 H21 . . 117.5
C20 C21 H21 . . 117.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O3 . 2.111(4)
Mn1 O1 . 2.121(4)
Mn1 O4 . 2.134(4)
Mn1 O2 . 2.145(5)
Mn1 N1 . 2.155(5)
Mn1 Mn1 2_666 3.0046(18)
Si2 C8 . 1.852(7)
Si2 C9 . 1.861(7)
Si2 C1 . 1.877(6)
Si2 C10 . 1.894(6)
O1 C2 . 1.256(8)
O2 C13 2_666 1.248(8)
O3 C2 2_666 1.273(8)
O4 C13 . 1.242(9)
N1 C21 . 1.288(9)
N1 C17 . 1.314(8)
C1 C5 . 1.388(8)
C1 C6 . 1.392(9)
C2 O3 2_666 1.273(8)
C2 C3 . 1.501(8)
C3 C4 . 1.365(9)
C3 C7 . 1.384(9)
C4 C5 . 1.390(8)
C4 H4 . 0.93
C5 H5 . 0.93
C6 C7 . 1.388(9)
C6 H6 . 0.93
C7 H7 . 0.93
C8 H8A . 0.96
C8 H8B . 0.96
C8 H8C . 0.96
C9 H9A . 0.96
C9 H9B . 0.96
C9 H9C . 0.96
C10 C12 . 1.386(9)
C10 C11 . 1.395(9)
C11 C15 1_465 1.387(9)
C11 H11 . 0.93
C12 C16 1_465 1.389(9)
C12 H12 . 0.93
C13 O2 2_666 1.248(8)
C13 C14 . 1.507(9)
C14 C15 . 1.370(9)
C14 C16 . 1.385(9)
C15 C11 1_645 1.387(9)
C15 H15 . 0.93
C16 C12 1_645 1.389(9)
C16 H16 . 0.93
C17 C18 . 1.378(10)
C17 H17 . 0.93
C18 C19 . 1.351(9)
C18 H18 . 0.93
C19 C20 . 1.352(10)
C19 C19 2_776 1.501(12)
C20 C21 . 1.392(11)
C20 H20 . 0.93
C21 H21 . 0.93
