Synthesis and Structural Characterization of a New Class of Macrocycles Based on a Cyclodiphosphazane Skeleton
Praveen Kommana; K. C. Kumara Swamy; Inorganic Chemistry 39 (2000) 4384–4385; doi:10.1021/ic000359o

data_4321406
_publ_section_title
;
 Synthesis and Structural Characterization of a New Class of Macrocycles
 Based on a Cyclodiphosphazane Skeleton
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4384
_journal_page_last               4385
_journal_paper_doi               10.1021/ic000359o
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C29.5 H40 Cl4 N2 O4 P2'
_chemical_formula_weight         690.38
_chemical_name_systematic
; 
 ? 
;
_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                 111.49(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.254(6)
_cell_length_b                   20.386(3)
_cell_length_c                   18.146(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6972(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.485
_diffrn_measured_fraction_theta_max 0.485
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7033
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.467
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6842
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0698P)^2^+4.6037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1651
_reflns_number_gt                3304
_reflns_number_total             6842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000359o_2.cif
_cod_data_source_block           Compound5
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+4.6037P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+4.6037P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6971(3)
_cod_original_formula_sum        'C29.50 H40 Cl4 N2 O4 P2'
_cod_database_code               4321406