Metalation studies of 3- and 4-pyridyloxycyclophosphazenes: metallamacrocycles to coordination polymers.
Chandrasekhar, Vadapalli; Narayanan, Ramakirushnan Suriya; Dalton transactions (Cambridge, England : 2003) 42 (2013) 6619–6632; doi:10.1039/c3dt33084b

data_7022819
_publ_section_title
;
 Metalation studies of 3- and 4-pyridyloxycyclophosphazenes:
 metallamacrocycles to coordination polymers.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6619
_journal_page_last               6632
_journal_paper_doi               10.1039/c3dt33084b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C64 H48 Cl8 Cu4 N14 O12 P6, 8(C H Cl3)'
_chemical_formula_sum            'C72 H56 Cl32 Cu4 N14 O12 P6'
_chemical_formula_weight         2883.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.250(3)
_cell_angle_beta                 77.262(3)
_cell_angle_gamma                81.256(3)
_cell_formula_units_Z            1
_cell_length_a                   13.015(2)
_cell_length_b                   13.723(2)
_cell_length_c                   15.691(2)
_cell_measurement_reflns_used    2588
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.31
_cell_measurement_theta_min      2.34
_cell_volume                     2667.5(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 0.980
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14859
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.740
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.361007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.254
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                6626
_reflns_number_total             10216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt33084b.txt
_cod_data_source_block           908590
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2667.6(7)
_cod_original_formula_sum        'C72 H56 Cl32 Cu4 N14 O12 P6 '
_cod_database_code               7022819