H-bonded adducts of [2,4,6-{(C10H21O)3C6H2NH}3C3N3] with [LnM{PPh2(C6H4CO2H)}] displaying Columnar Mesophases at Room Temperature.
Miguel-Coello, Ana B; Bardají, Manuel; Coco, Silverio; Donnio, Bertrand; Heinrich, Benoît; Espinet, Pablo; Inorganic chemistry 53 (2014) 10893–10902; doi:10.1021/ic501039n

data_4341182
_publ_section_title
;
 H-bonded adducts of [2,4,6-{(C10H21O)3C6H2NH}3C3N3] with
 [LnM{PPh2(C6H4CO2H)}] displaying Columnar Mesophases at Room Temperature.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10893
_journal_page_last               10902
_journal_paper_doi               10.1021/ic501039n
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C25.5 H15 Cr O7 P'
_chemical_formula_weight         516.34
_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                78.135(4)
_cell_angle_beta                 74.224(4)
_cell_angle_gamma                88.521(4)
_cell_formula_units_Z            4
_cell_length_a                   10.9729(5)
_cell_length_b                   14.6769(7)
_cell_length_c                   15.7818(8)
_cell_measurement_reflns_used    5632
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.9065
_cell_measurement_theta_min      2.9713
_cell_volume                     2392.4(2)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14476
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         75.08
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    4.951
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.2900
_exptl_crystal_size_mid          0.1851
_exptl_crystal_size_min          0.0831
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0586P)^2^+0.2378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                7012
_reflns_number_total             9356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501039n_si_002.cif
_cod_data_source_block           rf8an
_cod_depositor_comments
'Adding full bibliography for 4341179--4341182.cif.'
_cod_original_formula_sum        'C25.50 H15 Cr O7 P'
_cod_database_code               4341182