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_7109130
_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 H228 Co4 Dy10 N10 O66 P12, C4 N2 H6'
_chemical_formula_sum            'C128 H234 Co4 Dy10 N12 O66 P12'
_chemical_formula_weight         5229.68
_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                108.0775(13)
_cell_angle_beta                 101.8103(13)
_cell_angle_gamma                92.1947(12)
_cell_formula_units_Z            2
_cell_length_a                   17.0917(3)
_cell_length_b                   20.9589(3)
_cell_length_c                   30.4298(4)
_cell_measurement_reflns_used    32178
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      26.3341
_cell_measurement_theta_min      1.5677
_cell_volume                     10082.3(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 0.9971
_diffrn_measured_fraction_theta_max 0.9971
_diffrn_measurement_details
;
1 omega 2.20 182.01 0.2997 12.5000
omega____ theta____ kappa____ phi______ frames
- 28.0000 73.8962 -25.8019 600
2 omega 2.20 182.01 0.2997 12.5000
omega____ theta____ kappa____ phi______ frames
- 28.0000 73.8962 94.1981 600
3 omega 2.20 182.01 0.2997 12.5000
omega____ theta____ kappa____ phi______ frames
- 28.0000 73.8962 214.1962 600
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0180411000
_diffrn_orient_matrix_UB_12      -0.0117603000
_diffrn_orient_matrix_UB_13      -0.0196473000
_diffrn_orient_matrix_UB_21      0.0320217000
_diffrn_orient_matrix_UB_22      -0.0099981000
_diffrn_orient_matrix_UB_23      0.0144019000
_diffrn_orient_matrix_UB_31      -0.0216433000
_diffrn_orient_matrix_UB_32      -0.0323176000
_diffrn_orient_matrix_UB_33      -0.0063832000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.1084
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            79235
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.57
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89281
_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            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.075
_refine_diff_density_min         -2.169
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1877
_refine_ls_number_reflns         40171
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0868
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+214.8815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1944
_reflns_number_gt                26012
_reflns_number_total             40171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40907d.txt
_cod_data_source_block           Co4Dy10P12
_cod_database_code               7109130