Exo-metal coordination by a tricyclic [{P(μ-N-2-NC5H4)}2(μ-O)]2 dimer in [{P(μ-N-2-NC5H4)}2(μ-O)]2{CuCl·(C5H5N)2}4 {2-NC5H4 = 2-pyridyl, C5H5N = pyridine)
Bond, Andrew D.; Doyle, Emma L.; García, Felipe; Kowenicki, Richard A.; McPartlin, Mary; Riera, Lucía; Wright, Dominic S.; Chemical Communications (Cambridge, United Kingdom)  (2003) 2990–2991; doi:10.1039/b309842g

data_7113605
_publ_section_title
;
 Exo-metal coordination by a tricyclic [{P(\m-N-2-NC5H4)}2(\m-O)]2 dimer in
 [{P(\m-N-2-NC5H4)}2(\m-O)]2{CuCl&#x00B7;(C5H5N)2}4 {2-NC5H4 =
 2-pyridyl, C5H5N = pyridine)
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   24
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2990
_journal_page_last               2991
_journal_paper_doi               10.1039/b309842g
_journal_year                    2003
_chemical_formula_sum            'C30 H30 Cl2 Cu N6'
_chemical_formula_weight         609.04
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8453(3)
_cell_length_b                   14.2813(3)
_cell_length_c                   16.8855(5)
_cell_measurement_reflns_used    6968
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2856.46(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    teXsan
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15146
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.299
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+5.8840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                1082
_reflns_number_total             1635
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103907
_cod_data_source_file            b309842g.txt
_cod_data_source_block           dw0240
_cod_original_sg_symbol_H-M      Ccca
_cod_database_code               7113605