Synthesis, Structure, and Two-Photon Absorption Studies of a Phosphorus-Based Tris Hydrazone Ligand (S)P[N(Me)N=CH-C6H3-2-OH-4-N(CH2CH3)2]3 and Its Metal Complexes
Vadapalli Chandrasekhar; Ramachandran Azhakar; Balasubramanian Murugesapandian; Tapas Senapati; Prasenjit Bag; Mrituanjay D. Pandey; Sandeep Kumar Maurya; Debabrata Goswami; Inorganic Chemistry 49 (2010) 4008–4016; doi:10.1021/ic901531e

data_4315427
_publ_contact_author_address
;Head, Department of Chemistry
Indian Institute of Technology Kanpur
Kanpur 208016
Uttarpradesh
India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91-512-259 7436'
_publ_contact_author_name        'Prof. V. Chandrasekhar'
_publ_contact_author_phone       '+91-512-259 7259'
_publ_section_title
;
 Synthesis, Structure, and Two-Photon Absorption Studies of a
 Phosphorus-Based Tris Hydrazone Ligand
 (S)P[N(Me)N=CH-C6H3-2-OH-4-N(CH2CH3)2]3 and Its Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4008
_journal_page_last               4016
_journal_paper_doi               10.1021/ic901531e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C151 H218 Cl14 N36 Ni6 O12 P4 S4'
_chemical_formula_weight         3830.29
_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                 96.4330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.3154(8)
_cell_length_b                   23.5940(10)
_cell_length_c                   21.7367(10)
_cell_measurement_reflns_used    4855
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.88
_cell_measurement_theta_min      2.28
_cell_volume                     8824.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49463
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  0.9709
_exptl_absorpt_correction_T_min  0.9259
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4004
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.413
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         17316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1986
_reflns_number_gt                10116
_reflns_number_total             17316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901531e_si_002_4.cif
_cod_data_source_block           Complex-5
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-01-03

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315427