Dehydrogenative coupling of phenanthroline under hydrothermal conditions: crystal structure of a novel layered vanadate complex constructed of 4,8,10-net sheets: [(2,2′-biphen)Co]V3O8.5
Liu, Cai-Ming; Gao, Song; Kou, Hui-Zhong; Chemical Communications  (2001) 1670–; doi:10.1039/b103304m

data_7115051
_publ_section_title
;
 Dehydrogenative coupling of phenanthroline under hydrothermal conditions:
 crystal structure of a novel layered vanadate complex constructed of
 4,8,10-net sheets: [(2,2&#x2032;-biphen)Co]V3O8.5
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1670
_journal_paper_doi               10.1039/b103304m
_journal_year                    2001
_chemical_formula_sum            'C24 H14 Co N4 O8.5 V3'
_chemical_formula_weight         706.14
_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                 103.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.660(4)
_cell_length_b                   18.430(4)
_cell_length_c                   13.640(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4811.7(19)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       'Nonius Kappa CCD'
_computing_data_reduction        'HKL Denzo & Maxus'
_computing_molecular_graphics    'Siemens SHELXTL (1990)'
_computing_publication_material  'Siemens SHELXL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'NONIUS Kappa CCD'
_diffrn_measurement_method       CCD
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6778
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    1.870
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0551P)^2^+14.6957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                5750
_reflns_number_total             6778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103304m.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4811.7(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C24 H14 Co N4 O8.50 V3'
_cod_database_code               7115051