Tethered Pyrazolyl Phosphinate: Pyrazolyl-N- and Phosphoryl-O-Metal Coordination in Ph2P(O){OCH2CH2(3,5-Me2Pz)}
Savariraj Kingsley; Vadapalli Chandrasekhar; Christopher D. Incarvito; Matthew K. Lam; Arnold L. Rheingold; Inorganic Chemistry 40 (2001) 5890–5896; doi:10.1021/ic010454c

data_4320476
_publ_contact_author
;
       Chandrasekhar. V
       Department of Chemistry
       IIT, Kanpur 208 016
       India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91 512 597 436'
_publ_contact_author_phone       '+91 512 597 617'
_publ_section_title
;
 Tethered Pyrazolyl Phosphinate: Pyrazolyl-N- and Phosphoryl-O-Metal
 Coordination in Ph2P(O){OCH2CH2(3,5-Me2Pz)}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5890
_journal_page_last               5896
_journal_paper_doi               10.1021/ic010454c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C19 H21 N2 O2 P, 0.5(H2 O)'
_chemical_formula_sum            'C19 H24 N2 O3.5 P'
_chemical_formula_weight         367.37
_chemical_melting_point          90
_chemical_name_common            Ligpo(1)
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.40(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.897(5)
_cell_length_b                   10.009(2)
_cell_length_c                   19.147(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     3907(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      253(2)
_diffrn_measured_fraction_theta_full 0.831
_diffrn_measured_fraction_theta_max 0.831
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.1777
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3457
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1509
_reflns_number_gt                2330
_reflns_number_total             2836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010454c_1.cif
_cod_data_source_block           Ligpo
_cod_depositor_comments
;
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 

2020-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C19 H21 N2 O2 P), 3(H2 O)'
_cod_original_formula_sum        'C38 H48 N4 O7 P2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     734.74
_cod_database_code               4320476