Synthesis, characterization and anti-diabetic assay of diorganotin(iv) azo-carboxylates: crystal structure and topological studies of azo-dicarboxylic acid ligand and its cyclic tetranuclear dimethyltin(iv) complex
Roy, Manojit; Roy, Subhadip; Singh, Keisham Surjit; Kalita, Janmoni; Singh, S. Sureshkumar; New J. Chem. 40 (2016) 1471–; doi:10.1039/C5NJ02637G

data_7055201
_publ_section_title
;
 Synthesis, characterization and anti-diabetic assay of diorganotin(iv)
 azo-carboxylates: crystal structure and topological studies of
 azo-dicarboxylic acid ligand and its cyclic tetranuclear dimethyltin(iv)
 complex
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1471
_journal_paper_doi               10.1039/C5NJ02637G
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C36 H40 N4 O12 Sn4'
_chemical_formula_sum            'C36 H40 N4 O12 Sn4'
_chemical_formula_weight         1195.48
_chemical_name_systematic
;
 ? 
;
_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_date             2015-04-24
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.02.26 svn.r3159 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2015-09-17 deposited with the CCDC.
2015-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                88.004(2)
_cell_angle_beta                 69.650(2)
_cell_angle_gamma                79.051(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5462(3)
_cell_length_b                   9.7820(3)
_cell_length_c                   11.8061(4)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.02
_cell_measurement_theta_min      2.32
_cell_volume                     1014.26(6)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0213
_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       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26656
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.122
_exptl_absorpt_coefficient_mu    2.499
_exptl_absorpt_correction_T_max  0.5299
_exptl_absorpt_correction_T_min  0.4712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.00150(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4654
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0284
_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/[\s^2^(Fo^2^)+(0.0142P)^2^+2.3869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3824
_reflns_number_total             4654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02637g2.cif
_cod_data_source_block           kss15
_cod_depositor_comments
'Adding full bibliography for 7055200--7055201.cif.'
_cod_database_code               7055201
_shelx_estimated_absorpt_t_max   0.521
_shelx_estimated_absorpt_t_min   0.475
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid body (RIGU) restrains
 C2, O1, O2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, O1A, O2A, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(Sn2A)=Sof(O1A)=Sof(O2A)=Sof(C1A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(Sn2B)=Sof(O1)=Sof(O2)=Sof(C1)=Sof(C17B)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C13(H13)
4.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17B(H17A,H17B,H17C), C18B(H18A,
 H18B,H18C), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F)
4.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'