Crystal structure of pentakis(ethylenediamine-κ^2^<i>N</i>,<i>N</i>')lanthanum(III) trichloride‒ethylenediamine‒dichloromethane (1/1/1)
Sartain, Hope T.; Staples, Richard J.; Biros, Shannon M.; Acta Crystallographica Section E 70 (2014) 424–426; doi:10.1107/S1600536814023289

data_2240136
_publ_section_title
;
 Crystal structure of
 pentakis(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')lanthanum(III)
 trichloride--ethylenediamine--dichloromethane (1/1/1)
;
_journal_coeditor_code           PK2532
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              424
_journal_page_last               426
_journal_paper_doi               10.1107/S1600536814023289
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[La (C2 H8 N2)5] Cl3, C2 H8 N2, C H2 Cl2 '
_chemical_formula_moiety
'C10 H40 La N10 3+, 3(Cl -), C2 H8 N2, C H2 Cl2'
_chemical_formula_sum            'C13 H50 Cl5 La N12'
_chemical_formula_weight         690.78
_chemical_name_systematic
;Pentakis(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')lanthanum(III)
trichloride--ethylenediamine--dichloromethane (1/1/1)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.1560(9)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.8070(7)
_cell_length_b                   14.6530(12)
_cell_length_c                   22.1110(18)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      26.029
_cell_measurement_theta_min      2.308
_cell_volume                     2851.4(4)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2007)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009, 2014)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24978
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.035
_diffrn_reflns_theta_min         1.668
_exptl_absorpt_coefficient_mu    1.993
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.484
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5609
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+1.7999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                4502
_reflns_number_total             5609
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2532sup1.cf
_cod_data_source_block           I
_cod_database_code               2240136
_cod_database_fobs_code          2240136