4,4'-Methylenediphenol–4,4'-bipyridine (2/3): decarboxylation of 5,5'-methylenedisalicylic acid under hydrothermal conditions
Zhang, Zhi-Hui; Tan, Xue; Chen, Sheng-Chun; Acta Crystallographica Section C 65 (2009) o457–o459; doi:10.1107/S0108270109030832

data_2017314
_publ_section_title
;
 4,4'-Methylenediphenol--4,4'-bipyridine (2/3): decarboxylation of
 5,5'-methylenedisalicylic acid under hydrothermal conditions
;
_journal_coeditor_code           SQ3200
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o457
_journal_page_last               o459
_journal_paper_doi               10.1107/S0108270109030832
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '2 C13 H12 O2 , 3 C10 H8 N2'
_chemical_formula_moiety         '2 C13 H12 O2 , 3 C10 H8 N2'
_chemical_formula_sum            'C56 H48 N6 O4'
_chemical_formula_weight         869.00
_chemical_name_systematic
;
4,4'-Methylenediphenol--4,4'-bipyridine (2/3)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 127.755(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.606(2)
_cell_length_b                   5.7354(6)
_cell_length_c                   25.4316(18)
_cell_measurement_reflns_used    1921
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      21.53
_cell_measurement_theta_min      2.63
_cell_volume                     2261.0(4)
_computing_cell_refinement       'APEX2 (Bruker, 2003) and SAINT (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2005)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11614
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.988000
_exptl_absorpt_correction_T_min  0.981191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.146
_refine_ls_extinction_coef       0.0044(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.4007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                2727
_reflns_number_total             3976
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3200.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2017314
_cod_database_fobs_code          2017314