#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:09:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179096 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/58/4305857.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_4305857
loop_
_publ_author_name
'Pampa Mukherjee'
'Michael G. B. Drew'
'Marta Estrader'
'Ashutosh Ghosh'
_publ_section_title
;
Coordination-Driven Self-Assembly of a Novel Carbonato-Bridged
Heteromolecular Neutral Nickel(II) Triangle by Atmospheric CO2 Fixation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7784
_journal_page_last               7791
_journal_paper_doi               10.1021/ic800786s
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C24 H32 N6 Ni O2 S2'
_chemical_formula_weight         559.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 97.414(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9536(15)
_cell_length_b                   7.4582(8)
_cell_length_c                   14.9241(8)
_cell_measurement_reflns_used    8324
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.34
_cell_volume                     1319.4(2)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.1234
_diffrn_reflns_av_sigmaI/netI    0.1381
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8325
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.594
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1771
_refine_ls_R_factor_gt           0.1130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.1509P)²+16.0193P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3372
_refine_ls_wR_factor_ref         0.3746
_reflns_number_gt                2298
_reflns_number_total             3810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800786s-file001_2.cif
_cod_data_source_block           2
_cod_database_code               4305857
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C12 C 0.6020(7) 0.2838(12) 0.3604(5) 0.0314(17) Uani 1 1 d . . .
C13 C 0.6544(8) 0.1245(13) 0.3373(5) 0.0379(19) Uani 1 1 d . . .
H13 H 0.6811 0.0442 0.3827 0.046 Uiso 1 1 calc R . .
C14 C 0.6670(7) 0.0846(13) 0.2497(5) 0.0363(18) Uani 1 1 d . . .
H14 H 0.6998 -0.0236 0.2364 0.044 Uiso 1 1 calc R . .
C15 C 0.6312(8) 0.2038(13) 0.1804(5) 0.038(2) Uani 1 1 d . . .
H15 H 0.6421 0.1792 0.1211 0.046 Uiso 1 1 calc R . .
C16 C 0.5795(8) 0.3580(13) 0.2019(5) 0.038(2) Uani 1 1 d . . .
H16 H 0.5552 0.4381 0.1557 0.046 Uiso 1 1 calc R . .
C17 C 0.5613(7) 0.4016(12) 0.2898(5) 0.0291(16) Uani 1 1 d . . .
C18 C 0.5111(7) 0.5733(12) 0.3035(5) 0.0310(16) Uani 1 1 d . . .
H18 H 0.5035 0.6506 0.2541 0.037 Uiso 1 1 calc R . .
C20 C 0.4292(8) 0.8130(11) 0.3665(5) 0.0342(18) Uani 1 1 d . . .
H20A H 0.4774 0.8868 0.3341 0.041 Uiso 1 1 calc R . .
H20B H 0.4294 0.8640 0.4263 0.041 Uiso 1 1 calc R . .
C21 C 0.3099(8) 0.8189(12) 0.3174(5) 0.0359(19) Uani 1 1 d . . .
H21A H 0.3117 0.7806 0.2555 0.043 Uiso 1 1 calc R . .
H21B H 0.2841 0.9423 0.3156 0.043 Uiso 1 1 calc R . .
C22 C 0.2243(7) 0.7043(12) 0.3583(5) 0.0329(17) Uani 1 1 d . . .
H22A H 0.1508 0.7163 0.3227 0.039 Uiso 1 1 calc R . .
H22B H 0.2464 0.5793 0.3575 0.039 Uiso 1 1 calc R . .
N23 N 0.2174(6) 0.7616(9) 0.4526(4) 0.0311(14) Uani 1 1 d . . .
H23A H 0.2077 0.8813 0.4535 0.037 Uiso 1 1 calc R . .
H23B H 0.2833 0.7364 0.4865 0.037 Uiso 1 1 calc R . .
C24 C 0.1241(8) 0.6744(13) 0.4942(6) 0.040(2) Uani 1 1 d . . .
H24A H 0.1272 0.7120 0.5560 0.060 Uiso 1 1 calc R . .
H24B H 0.1323 0.5465 0.4919 0.060 Uiso 1 1 calc R . .
H24C H 0.0529 0.7085 0.4614 0.060 Uiso 1 1 calc R . .
N31 N 0.3588(6) 0.3367(10) 0.4655(4) 0.0355(16) Uani 1 1 d . . .
C32 C 0.2694(7) 0.2669(10) 0.4524(5) 0.0288(16) Uani 1 1 d . . .
O11 O 0.5966(5) 0.3190(8) 0.4459(3) 0.0336(13) Uani 1 1 d . . .
S33 S 0.14501(19) 0.1778(3) 0.43440(14) 0.0355(5) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.5000 0.5000 0.0273(4) Uani 1 2 d S . .
N19 N 0.4758(6) 0.6327(9) 0.3753(4) 0.0284(14) 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
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
_geom_angle_publ_flag
O11 C12 C13 119.2(7) . . ?
O11 C12 C17 123.1(8) . . ?
C13 C12 C17 117.6(7) . . ?
C14 C13 C12 121.8(8) . . ?
C13 C14 C15 120.7(8) . . ?
C16 C15 C14 118.1(7) . . ?
C15 C16 C17 123.2(8) . . ?
C16 C17 C12 118.5(8) . . ?
C16 C17 C18 117.3(7) . . ?
C12 C17 C18 123.9(6) . . ?
N19 C18 C17 127.9(7) . . ?
N19 C20 C21 113.3(7) . . ?
C20 C21 C22 115.4(6) . . ?
N23 C22 C21 110.0(7) . . ?
C22 N23 C24 113.8(7) . . ?
C32 N31 Ni1 168.7(7) . . ?
N31 C32 S33 178.1(8) . . ?
C12 O11 Ni1 128.9(5) . . ?
O11 Ni1 O11 180.000(1) 3_666 . ?
O11 Ni1 N31 90.2(3) 3_666 . ?
O11 Ni1 N31 89.8(3) . . ?
O11 Ni1 N31 89.8(3) 3_666 3_666 ?
O11 Ni1 N31 90.2(3) . 3_666 ?
N31 Ni1 N31 180.0 . 3_666 ?
O11 Ni1 N19 88.9(2) 3_666 3_666 ?
O11 Ni1 N19 91.1(2) . 3_666 ?
N31 Ni1 N19 87.6(3) . 3_666 ?
N31 Ni1 N19 92.4(3) 3_666 3_666 ?
O11 Ni1 N19 91.1(2) 3_666 . ?
O11 Ni1 N19 88.9(2) . . ?
N31 Ni1 N19 92.4(3) . . ?
N31 Ni1 N19 87.6(3) 3_666 . ?
N19 Ni1 N19 179.999(1) 3_666 . ?
C18 N19 C20 114.1(7) . . ?
C18 N19 Ni1 123.9(6) . . ?
C20 N19 Ni1 121.6(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C12 O11 1.312(8) . ?
C12 C13 1.406(12) . ?
C12 C17 1.410(11) . ?
C13 C14 1.367(10) . ?
C14 C15 1.389(13) . ?
C15 C16 1.363(13) . ?
C16 C17 1.395(9) . ?
C17 C18 1.440(12) . ?
C18 N19 1.281(9) . ?
C20 N19 1.455(11) . ?
C20 C21 1.518(13) . ?
C21 C22 1.521(12) . ?
C22 N23 1.484(9) . ?
N23 C24 1.494(10) . ?
N31 C32 1.183(11) . ?
N31 Ni1 2.091(8) . ?
C32 S33 1.619(9) . ?
O11 Ni1 2.012(5) . ?
Ni1 O11 2.012(5) 3_666 ?
Ni1 N31 2.091(8) 3_666 ?
Ni1 N19 2.095(6) 3_666 ?
Ni1 N19 2.095(6) . ?
