#------------------------------------------------------------------------------
#$Date: 2019-11-23 14:07:48 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233558 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/90/4349053.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_4349053
loop_
_publ_author_name
'Wallen, Christian M.'
'Wielizcko, Marika'
'Bacsa, John'
'Scarborough, Christopher C.'
_publ_section_title
;
 Heterotrimetallic sandwich complexes supported by sulfonamido ligands
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              142
_journal_paper_doi               10.1039/C5QI00233H
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C36 H78 Ca1 Co2 N8 O12 S6'
_chemical_formula_sum            'C36 H78 Ca Co2 N8 O12 S6'
_chemical_formula_weight         1165.36
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-28
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-30 deposited with the CCDC.
2015-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.601(3)
_cell_length_b                   12.601(3)
_cell_length_c                   29.273(8)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.920
_cell_measurement_theta_min      2.328
_cell_volume                     4025.4(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            17386
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.068
_diffrn_reflns_theta_min         2.087
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.4389
_exptl_absorpt_correction_T_min  0.3299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0977 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.7517.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0595P)²+1.4018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3518
_reflns_number_total             4461
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5qi00233h2.cif
_cod_data_source_block           cmw_03_020
_cod_original_cell_volume        4025(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4349053
_shelxl_version_number           2013-4
_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_max   0.896
_shelx_estimated_absorpt_t_min   0.683
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, {H5B,H5A} of C5
 At 1.2 times of:
  {H1A,H1B} of C1, {H2BA,H2BB} of C2B, {H1BA,H1BB} of C1B, {H2B,H2A} of C2
2. Restrained distances
 N1-C1 \\sim N1-C1B
 with sigma of 0.002
 C2B-C1B \\sim C2-C1
 with sigma of 0.002
 N2-C2 \\sim N2-C2B
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C1 \\sim C1B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C2B \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1B) = Uanis(C1)
Uanis(C2B) = Uanis(C2)
4. Rigid body (RIGU) restrains
 N2, C2B, C2, C1, C1B, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2B)=Sof(H2A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2B,H2A), C1B(H1BA,H1BB), C2B(H2BA,H2BB)
6.b Idealised Me refined as rotating group:
 C4(H4A,H4C,H4B), C6(H6B,H6A,H6C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id CMW-03-020
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-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'
'-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'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.12734(18) 0.0871(2) 0.29225(6) 0.0266(4) Uani 0.748(3) 1 d D U . A -1
H1A H 0.1259 0.1214 0.2620 0.032 Uiso 0.748(3) 1 calc R . . A -1
H1B H 0.1741 0.0435 0.2894 0.032 Uiso 0.748(3) 1 calc R . . A -1
C2 C 0.1895(2) 0.19094(19) 0.32714(5) 0.0275(4) Uani 0.748(3) 1 d D U . A -1
H2B H 0.2785 0.2402 0.3209 0.033 Uiso 0.748(3) 1 calc R . . A -1
H2A H 0.1542 0.2455 0.3256 0.033 Uiso 0.748(3) 1 calc R . . A -1
C1B C 0.1073(4) 0.1229(3) 0.29827(18) 0.0266(4) Uani 0.252(3) 1 d D U . A -2
H1BA H 0.0831 0.1853 0.3041 0.032 Uiso 0.252(3) 1 calc R . . A -2
H1BB H 0.1291 0.1279 0.2655 0.032 Uiso 0.252(3) 1 calc R . . A -2
C2B C 0.2214(4) 0.1551(7) 0.32673(10) 0.0275(4) Uani 0.252(3) 1 d D U . A -2
H2BA H 0.2551 0.1009 0.3196 0.033 Uiso 0.252(3) 1 calc R . . A -2
H2BB H 0.2861 0.2417 0.3225 0.033 Uiso 0.252(3) 1 calc R . . A -2
C3 C 0.36798(13) 0.18401(14) 0.42740(5) 0.0250(3) Uani 1 1 d . . . . .
C4 C 0.45144(17) 0.23030(19) 0.38538(7) 0.0430(4) Uani 1 1 d . . . . .
H4A H 0.4080 0.1794 0.3589 0.065 Uiso 1 1 calc GR . . . .
H4C H 0.5256 0.2256 0.3911 0.065 Uiso 1 1 calc GR . . . .
H4B H 0.4741 0.3155 0.3792 0.065 Uiso 1 1 calc GR . . . .
C5 C 0.31899(16) 0.04749(16) 0.43444(6) 0.0311(3) Uani 1 1 d . . . . .
H5B H 0.271(2) 0.021(2) 0.4607(8) 0.047 Uiso 1 1 d R . . . .
H5A H 0.271(2) 0.002(2) 0.4099(9) 0.047 Uiso 1 1 d R . . . .
C6 C 0.43493(17) 0.25587(19) 0.47016(7) 0.0409(4) Uani 1 1 d . . . . .
H6B H 0.4601 0.3425 0.4660 0.061 Uiso 1 1 calc GR . . . .
H6A H 0.5075 0.2480 0.4753 0.061 Uiso 1 1 calc GR . . . .
H6C H 0.3801 0.2232 0.4966 0.061 Uiso 1 1 calc GR . . . .
N1 N 0.0000 0.0000 0.30721(6) 0.0220(3) Uani 1 3 d DS TU P . .
N2 N 0.16760(11) 0.13226(12) 0.37351(3) 0.0242(2) Uani 1 1 d D U . . .
O1 O 0.15613(8) 0.14992(9) 0.45574(3) 0.01764(16) Uani 1 1 d . . . . .
O2 O 0.28909(10) 0.33815(9) 0.41204(3) 0.0253(2) Uani 1 1 d . . . . .
S1 S 0.23948(3) 0.20780(3) 0.41686(2) 0.01747(7) Uani 1 1 d . . . . .
Ca1 Ca 0.0000 0.0000 0.5000 0.01352(10) Uani 1 6 d S T P . .
Co2 Co 0.0000 0.0000 0.37878(2) 0.01600(7) Uani 1 3 d S T P A .
H5C H 0.392(2) 0.037(2) 0.4381(8) 0.046(6) Uiso 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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
S S 0.1246 0.1234 '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
H1A C1 H1B 108.2 . .
C2 C1 H1A 109.7 . .
C2 C1 H1B 109.7 . .
N1 C1 H1A 109.7 . .
N1 C1 H1B 109.7 . .
N1 C1 C2 109.66(15) . .
C1 C2 H2B 110.3 . .
C1 C2 H2A 110.3 . .
H2B C2 H2A 108.6 . .
N2 C2 C1 106.99(15) . .
N2 C2 H2B 110.3 . .
N2 C2 H2A 110.3 . .
H1BA C1B H1BB 107.5 . .
C2B C1B H1BA 108.5 . .
C2B C1B H1BB 108.5 . .
N1 C1B H1BA 108.5 . .
N1 C1B H1BB 108.5 . .
N1 C1B C2B 115.2(4) . .
C1B C2B H2BA 111.8 . .
C1B C2B H2BB 111.8 . .
H2BA C2B H2BB 109.5 . .
N2 C2B C1B 99.9(3) . .
N2 C2B H2BA 111.8 . .
N2 C2B H2BB 111.8 . .
C4 C3 S1 107.46(11) . .
C5 C3 C4 110.62(13) . .
C5 C3 C6 110.51(14) . .
C5 C3 S1 108.56(10) . .
C6 C3 C4 111.20(15) . .
C6 C3 S1 108.38(11) . .
C3 C4 H4A 109.5 . .
C3 C4 H4C 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4C 109.5 . .
H4A C4 H4B 109.5 . .
H4C C4 H4B 109.5 . .
C3 C5 H5B 110.0(15) . .
C3 C5 H5A 110.9(16) . .
C3 C5 H5C 106.5(14) . .
H5B C5 H5A 108(2) . .
H5B C5 H5C 110(2) . .
H5A C5 H5C 111(2) . .
C3 C6 H6B 109.5 . .
C3 C6 H6A 109.5 . .
C3 C6 H6C 109.5 . .
H6B C6 H6A 109.5 . .
H6B C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
C1 N1 Co2 107.14(9) . .
C1B N1 Co2 100.2(2) . .
C2 N2 S1 121.46(11) . .
C2 N2 Co2 110.41(10) . .
C2B N2 S1 123.7(2) . .
C2B N2 Co2 115.8(2) . .
S1 N2 Co2 120.48(6) . .
S1 O1 Ca1 159.82(6) . .
N2 S1 C3 109.19(7) . .
O1 S1 C3 105.14(6) . .
O1 S1 N2 105.77(6) . .
O2 S1 C3 106.87(7) . .
O2 S1 N2 113.62(7) . .
O2 S1 O1 115.82(6) . .
O1 Ca1 O1 88.06(3) 2 10_556
O1 Ca1 O1 91.94(3) 3 .
O1 Ca1 O1 88.06(3) 3 11_556
O1 Ca1 O1 88.06(3) 12_556 2
O1 Ca1 O1 91.94(3) 2 .
O1 Ca1 O1 91.94(3) 11_556 10_556
O1 Ca1 O1 180.00(3) 10_556 .
O1 Ca1 O1 91.94(3) 12_556 10_556
O1 Ca1 O1 180.0 11_556 2
O1 Ca1 O1 91.94(3) 3 2
O1 Ca1 O1 88.06(3) 3 10_556
O1 Ca1 O1 88.06(3) 12_556 .
O1 Ca1 O1 180.0 12_556 3
O1 Ca1 O1 91.94(3) 12_556 11_556
O1 Ca1 O1 88.06(3) 11_556 .
O1 Ca1 Co2 123.88(2) 12_556 .
O1 Ca1 Co2 123.88(2) 10_556 .
O1 Ca1 Co2 56.12(2) 2 .
O1 Ca1 Co2 123.88(2) 2 10_556
O1 Ca1 Co2 123.88(2) 11_556 .
O1 Ca1 Co2 123.88(2) 3 10_556
O1 Ca1 Co2 56.12(2) 3 .
O1 Ca1 Co2 56.12(2) 11_556 10_556
O1 Ca1 Co2 56.12(2) 10_556 10_556
O1 Ca1 Co2 56.12(2) . .
O1 Ca1 Co2 56.12(2) 12_556 10_556
O1 Ca1 Co2 123.88(2) . 10_556
Co2 Ca1 Co2 180.0 . 10_556
N1 Co2 Ca1 180.0 . .
N2 Co2 N1 85.43(3) 2 .
N2 Co2 N1 85.42(3) . .
N2 Co2 N1 85.43(3) 3 .
N2 Co2 N2 119.370(9) . 3
N2 Co2 N2 119.371(9) . 2
N2 Co2 N2 119.371(9) 3 2
N2 Co2 Ca1 94.57(3) 3 .
N2 Co2 Ca1 94.57(3) 2 .
N2 Co2 Ca1 94.58(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C1 C2 1.531(3) .
C1 N1 1.4866(19) .
C2 H2B 0.9900 .
C2 H2A 0.9900 .
C2 N2 1.5035(19) .
C1B H1BA 0.9900 .
C1B H1BB 0.9900 .
C1B C2B 1.531(3) .
C1B N1 1.483(3) .
C2B H2BA 0.9900 .
C2B H2BB 0.9900 .
C2B N2 1.491(3) .
C3 C4 1.532(2) .
C3 C5 1.523(2) .
C3 C6 1.528(2) .
C3 S1 1.8145(16) .
C4 H4A 0.9800 .
C4 H4C 0.9800 .
C4 H4B 0.9800 .
C5 H5B 0.93(2) .
C5 H5A 0.93(3) .
C5 H5C 1.00(3) .
C6 H6B 0.9800 .
C6 H6A 0.9800 .
C6 H6C 0.9800 .
N1 Co2 2.0949(19) .
N2 S1 1.5731(12) .
N2 Co2 1.9343(13) .
O1 S1 1.4712(9) .
O1 Ca1 2.3241(10) .
O2 S1 1.4428(11) .
Ca1 O1 2.3240(10) 3
Ca1 O1 2.3240(10) 10_556
Ca1 O1 2.3240(10) 2
Ca1 O1 2.3240(10) 12_556
Ca1 O1 2.3240(10) 11_556
Ca1 Co2 3.5486(10) .
Ca1 Co2 3.5486(10) 10_556
Co2 N2 1.9343(13) 3
Co2 N2 1.9343(13) 2
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
C1 C2 N2 C2B 63.8(5)
C1 C2 N2 S1 167.55(14)
C1 C2 N2 Co2 -42.89(19)
C2 C1 N1 C1B 45.4(5)
C2 C1 N1 Co2 -31.62(18)
C2 N2 S1 C3 -97.39(15)
C2 N2 S1 O1 149.92(14)
C2 N2 S1 O2 21.79(16)
C1B C2B N2 C2 -51.7(3)
C1B C2B N2 S1 -146.7(3)
C1B C2B N2 Co2 33.9(5)
C2B C1B N1 C1 -63.0(5)
C2B C1B N1 Co2 45.9(5)
C2B N2 S1 C3 -63.4(3)
C2B N2 S1 O1 -176.1(3)
C2B N2 S1 O2 55.8(3)
C4 C3 S1 N2 60.91(13)
C4 C3 S1 O1 174.01(11)
C4 C3 S1 O2 -62.37(13)
C5 C3 S1 N2 -58.76(12)
C5 C3 S1 O1 54.34(11)
C5 C3 S1 O2 177.96(10)
C6 C3 S1 N2 -178.82(11)
C6 C3 S1 O1 -65.73(13)
C6 C3 S1 O2 57.89(13)
N1 C1 C2 N2 48.9(2)
N1 C1B C2B N2 -53.8(6)
Ca1 O1 S1 C3 -87.98(17)
Ca1 O1 S1 N2 27.50(19)
Ca1 O1 S1 O2 154.30(16)
Co2 N2 S1 C3 116.05(9)
Co2 N2 S1 O1 3.36(10)
Co2 N2 S1 O2 -124.77(8)
