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_7055200
_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         'C14 H10 N2 O5, H2 O'
_chemical_formula_sum            'C14 H12 N2 O6'
_chemical_formula_weight         304.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.7027(14)
_cell_length_b                   3.8296(2)
_cell_length_c                   13.3781(7)
_cell_measurement_reflns_used    2455
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.02
_cell_measurement_theta_min      3.04
_cell_volume                     1368.05(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0605
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17479
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.891
_diffrn_reflns_theta_min         3.045
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.9699
_exptl_absorpt_correction_T_min  0.9563
_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    1.477
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 608 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.5(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2659
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.4649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                1672
_reflns_number_total             2659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02637g2.cif
_cod_data_source_block           kss12
_cod_depositor_comments
'Adding full bibliography for 7055200--7055201.cif.'
_cod_database_code               7055200
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.960
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.9 with sigma of 0.02
 H1WA-H1WB
 1.47 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C13(H13), C10(H10), C9(H9)
3.b Tetrahedral OH refined with riding coordinates:
 O1(H1), O5(H5A), O3(H3A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'