Heavier Group 2 Metal Complexes with Flexible Scorpionate Ligand based on 2-Mercaptopyridine
Panda, Tarun Kanti Kanti; Naktode, Kishor; Mallik, Bhabani S.; Nayek, Hari Pada; Reddy, Th Dhileep; RSC Adv.  (2015) –; doi:10.1039/C5RA04696C

data_7220672
_publ_section_title
;
 Heavier Group 2 Metal Complexes with Flexible Scorpionate Ligand based on
 2-Mercaptopyridine
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA04696C
_journal_year                    2015
_chemical_formula_moiety         'C32 H44 B2 Ba N4 O3 S4'
_chemical_formula_sum            'C32 H44 B2 Ba N4 O3 S4'
_chemical_formula_weight         819.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-28
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.05.19 svn.r3182 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2015-05-29 deposited with the CCDC.
2015-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 132.543(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7544(7)
_cell_length_b                   17.7876(6)
_cell_length_c                   20.3426(6)
_cell_measurement_reflns_used    5683
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.02
_cell_measurement_theta_min      2.95
_cell_volume                     3666.9(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_collection
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at zero, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12832
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.497
_diffrn_reflns_theta_max         26.497
_diffrn_reflns_theta_min         2.950
_exptl_absorpt_coefficient_mu    1.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84776
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7159
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6060
_reflns_number_total             7159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra04696c2.cif
_cod_data_source_block           4
_cod_database_code               7220672
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6469(11) 0.3531(11)
2. Fixed Uiso
 At 1.2 times of:
  All B(H,H) groups, All C(H) groups, All C(H,H) groups
3. Rigid body (RIGU) restrains
 O2, C28, C27, C26, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 B1(H1A,H1B), B2(H2A,H2B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
  C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              60025
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'