Molecular amino-phosphonate cobalt-lanthanide clusters
Eufemio Moreno Pineda; Floriana Tuna; Robin G. Pritchard; Andrew C. Regan; Richard E. P. Winpenny; Eric J. L. McInnes; Chem.Commun. 49 (2013) 3522–; doi:10.1039/c3cc40907d

data_7109131
_publ_section_title
;
 Molecular amino-phosphonate cobalt-lanthanide clusters
;
_journal_name_full               Chem.Commun.
_journal_page_first              3522
_journal_paper_doi               10.1039/c3cc40907d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C124 H214 Co4 Gd10 N10 O66 P12, 3(C2 H3 N)'
_chemical_formula_sum            'C130 H245 Co4 Gd10 N13 O66 P12'
_chemical_formula_weight         5226.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2012-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2012.11.06 svn.r2526, GUI svn.r4372)
;
_audit_update_record
;
2012-11-24 # Formatted by publCIF
;
_cell_angle_alpha                70.1022(12)
_cell_angle_beta                 84.5267(11)
_cell_angle_gamma                79.3776(12)
_cell_formula_units_Z            2
_cell_length_a                   18.2190(2)
_cell_length_b                   22.4563(3)
_cell_length_c                   27.5752(4)
_cell_measurement_reflns_used    42726
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3314
_cell_measurement_theta_min      1.5685
_cell_volume                     10420.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9977
_diffrn_measurement_details
;
1 omega 2.20 182.15 0.2999 20.0000
omega____ theta____ kappa____ phi______ frames
- 28.0000 73.8966 -25.8022 600
2 omega 2.20 182.15 0.2999 20.0000
omega____ theta____ kappa____ phi______ frames
- 28.0000 73.8966 94.1986 600
3 omega 2.20 182.15 0.2999 20.0000
omega____ theta____ kappa____ phi______ frames
- 28.0000 73.8966 214.1966 600
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0381970000
_diffrn_orient_matrix_UB_12      0.0036155000
_diffrn_orient_matrix_UB_13      -0.0028608000
_diffrn_orient_matrix_UB_21      -0.0084243000
_diffrn_orient_matrix_UB_22      0.0252427000
_diffrn_orient_matrix_UB_23      0.0106245000
_diffrn_orient_matrix_UB_31      0.0064018000
_diffrn_orient_matrix_UB_32      -0.0225524000
_diffrn_orient_matrix_UB_33      0.0250638000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.1421
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            84001
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.609
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5144
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.505
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1975
_refine_ls_number_reflns         42000
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_gt           0.0953
_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^)+(0.0656P)^2^+189.2302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2181
_reflns_number_gt                26513
_reflns_number_total             42000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40907d.txt
_cod_data_source_block           Co4Gd10P12
_cod_original_cell_volume        10420.1(2)
_cod_database_code               7109131