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_7022824
_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         'C34 H24 Cl2 Cu N5 O6 P3'
_chemical_formula_sum            'C34 H24 Cl2 Cu N5 O6 P3'
_chemical_formula_weight         825.93
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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_date             2013-02-11
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.470(7)
_cell_length_b                   11.331(2)
_cell_length_c                   24.468(5)
_cell_measurement_reflns_used    2943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.132
_cell_measurement_theta_min      2.327
_cell_volume                     9510(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24874
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.398261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0963 before and 0.0360 after correction.
The Ratio of minimum to maximum transmission is 0.3983.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1837
_reflns_number_gt                4710
_reflns_number_total             8820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt33084b.txt
_cod_data_source_block           908595
_cod_original_cell_volume        9510.1(3)
_cod_database_code               7022824
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H10 of C10, H15 of C15, H11 of C11, H16 of C16, H17 of C17, H14 of C14, H20
of C20, H22 of C22, H8 of C8, H21 of C21, H9 of C9, H23 of C23, H26 of C26,
H27 of C27, H28 of C28, H31 of C31, H29 of C29, H32 of C32, H33 of C33, H34
of C34, H3 of C3, H2 of C2, H4 of C4, H5 of C5
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34)
;