Isotypical N,N-dialkylcarbamato lanthanide complexes covering a range of 11 atomic numbers: direct experimental assessment of the lanthanide contraction in trivalent molecular compounds
Abram, Ulrich; Dell’Amico, Daniela Belli; Calderazzo, Fausto; Porta, Cinzia Della; Merigo, Alessandra; Englert, Ulli; Marchetti, Fabio; Chemical Communications  (1999) 2053–; doi:10.1039/a904792a

data_7110625
_publ_section_title
;
 Isotypical N,N-dialkylcarbamato lanthanide complexes covering a range of
 11 atomic numbers: direct experimental assessment of the lanthanide
 contraction in trivalent molecular compounds
;
_journal_issue                   20
_journal_name_full               'Chemical Communications'
_journal_page_first              2053
_journal_paper_doi               10.1039/a904792a
_journal_year                    1999
_chemical_formula_moiety         'Ho4 (O2 C N i-Pr2)12'
_chemical_formula_sum            'C98 H200 Ho4 N12 O24'
_chemical_formula_weight         2590.42
_chemical_name_systematic
; 
 Dodecakis(N,N-diisopropylcarbamato)tetraholmium(iii) 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.130(2)
_cell_length_b                   19.844(2)
_cell_length_c                   23.1310(10)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.029
_cell_measurement_theta_min      9.697
_cell_volume                     12770.3(18)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10120
_diffrn_reflns_theta_full        23.01
_diffrn_reflns_theta_max         23.01
_diffrn_reflns_theta_min         2.05
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.514
_exptl_absorpt_correction_T_max  0.4623
_exptl_absorpt_correction_T_min  0.3425
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5328
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+99.2485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                6711
_reflns_number_total             8868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904792asup1.cif
_cod_data_source_block           holcar
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        12770.3(17)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               7110625