Substituent directed selectivity in anion recognition by a new class of simple osmium-pyrazole derived receptors.
Das, Ankita; Mondal, Prasenjit; Dasgupta, Moumita; Kishore, Nand; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2605–2617; doi:10.1039/c5dt04538j

data_7037683
_publ_section_title
;
 Substituent directed selectivity in anion recognition by a new class of
 simple osmium-pyrazole derived receptors.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2605
_journal_page_last               2617
_journal_paper_doi               10.1039/c5dt04538j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C25 H24 Cl N6 Os, Cl O4'
_chemical_formula_sum            'C25 H24 Cl2 N6 O4 Os'
_chemical_formula_weight         733.60
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_date             2015-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-16 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.401(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.017(8)
_cell_length_b                   11.932(5)
_cell_length_c                   15.605(8)
_cell_measurement_reflns_used    5012
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.10
_cell_measurement_theta_min      3.10
_cell_volume                     2566(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ORTEP
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_unetI/netI     0.0962
_diffrn_reflns_laue_measured_fraction_full 0.972
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17428
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.139
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.223
_exptl_absorpt_correction_T_max  0.4215
_exptl_absorpt_correction_T_min  0.4215
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4507
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0309P)^2^+5.1499P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3869
_reflns_number_total             4507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04538j2.cif
_cod_data_source_block           2ClO4
_cod_depositor_comments
'Adding full bibliography for 7037682--7037683.cif.'
_cod_database_code               7037683
_shelxl_version_number           2012-9
_shelx_estimated_absorpt_t_max   0.421
_shelx_estimated_absorpt_t_min   0.421
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C13) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.001
Uanis(C23) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C3)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C25(H25), C15(H15), C16(H16), C14(H14), C6(H6), C9(H9), C3(H3),
 C7(H7), C23(H23), C17(H17), C22(H22), C24(H24), C8(H8), C12(H12), C19(H19),
 C18(H18), C13(H13)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              98869
_shelx_hkl_checksum              19320
_olex2_submission_special_instructions 'No special instructions were received'