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_7109132
_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         'C100 H186 Co6 Gd4 N8 Na2 O44 P6, 2(C2 H3 N)'
_chemical_formula_sum            'C104 H192 Co6 Gd4 N10 Na2 O44 P6'
_chemical_formula_weight         3501.06
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2012.11.06 svn.r2526, GUI svn.r4372)
;
_audit_update_record
;
2012-12-06 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.274(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.8683(5)
_cell_length_b                   27.0973(8)
_cell_length_c                   19.4683(6)
_cell_measurement_reflns_used    15774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3285
_cell_measurement_theta_min      1.8769
_cell_volume                     7746.5(4)
_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 0.9944
_diffrn_measured_fraction_theta_max 0.9944
_diffrn_measurement_details
;
1 omega 2.20 182.15 0.2999 1.0000
omega____ theta____ kappa____ phi______ frames
- 28.0000 73.8966 -25.8022 600
2 omega 2.20 132.66 0.2999 1.0000
omega____ theta____ kappa____ phi______ frames
- 28.0000 73.8966 64.1977 435
3 omega 2.20 71.18 0.2999 1.0000
omega____ theta____ kappa____ phi______ frames
- 28.0000 73.8966 154.1977 230
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0241310000
_diffrn_orient_matrix_UB_12      -0.0124463000
_diffrn_orient_matrix_UB_13      0.0338303000
_diffrn_orient_matrix_UB_21      -0.0316249000
_diffrn_orient_matrix_UB_22      0.0088995000
_diffrn_orient_matrix_UB_23      0.0148378000
_diffrn_orient_matrix_UB_31      -0.0274191000
_diffrn_orient_matrix_UB_32      -0.0212248000
_diffrn_orient_matrix_UB_33      -0.0136420000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42633
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.88
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89380
_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            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.520
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         15760
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+45.6864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                12162
_reflns_number_total             15760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40907d.txt
_cod_data_source_block           Co6Gd4P6
_cod_database_code               7109132