Synthesis and characterisation of the ethylene bridged permethylindenyl cerium complex [(EBI*)CeI(THF)].
Ransom, Paul; Arnold, Thomas A. Q.; Thompson, Amber L.; Buffet, Jean-Charles; O'Hare, Dermot; Dalton transactions (Cambridge, England : 2003) 41 (2012) 11267–11269; doi:10.1039/c2dt31439h

data_7020396
_publ_section_title
;
 Synthesis and characterisation of the ethylene bridged permethylindenyl
 cerium complex [(EBI*)CeI(THF)].
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11267
_journal_page_last               11269
_journal_paper_doi               10.1039/c2dt31439h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C36 H48 Ce1 I1 O1'
_chemical_formula_sum            'C36 H48 Ce I O'
_chemical_formula_weight         763.80
_chemical_melting_point          ?
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             12-06-30
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.2981(1)
_cell_length_b                   19.2885(2)
_cell_length_c                   35.5339(4)
_cell_measurement_reflns_used    71481
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     6372.88(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.088
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            51825
_diffrn_reflns_theta_full        26.629
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         5.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Multi-scan from symmetry-related measurements using
Sortav (Blessing 1995).
;
_exptl_crystal_colour            clear_intense_orange
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3064.000
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.90
_refine_diff_density_min         -1.81
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9596
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7182
_refine_ls_number_restraints     180
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.0010361
_refine_ls_shift/su_mean         0.0000461
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
10.7 14.9 7.38 1.91
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1222
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1222
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                4811
_reflns_number_total             7182
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.08
_oxford_diffrn_Wilson_scale      518.08
_oxford_refine_ls_r_factor_ref   0.0894
_oxford_refine_ls_scale          0.063873(12)
_oxford_reflns_number_all        7182
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 5566
_cod_data_source_file            c2dt31439h.txt
_cod_data_source_block           meso-[(EBI*)CeI(THF)]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_atom_sites_solution_primary'
value 'Other' changed to 'other' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C36 H48 Ce1 I1 O1'
_cod_database_code               7020396
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
EQUIV PART(1001,OCC) PART(1002,OCC)
WEIGHT -1 PART(1002,OCC)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE C ( 4,X'S) H ( 42,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S)
RIDE C ( 6,X'S) H ( 62,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S)
RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) H ( 323,X'S)
RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S)
RIDE C ( 35,X'S) H ( 352,X'S) H ( 351,X'S) H ( 353,X'S)
RIDE C ( 36,X'S) H ( 362,X'S) H ( 361,X'S) H ( 363,X'S)
RIDE C ( 37,X'S) H ( 371,X'S) H ( 373,X'S) H ( 372,X'S)
RIDE C ( 38,X'S) H ( 381,X'S) H ( 383,X'S) H ( 382,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) H ( 433,X'S)
RIDE C ( 45,X'S) H ( 451,X'S) H ( 452,X'S) H ( 453,X'S)
RIDE C ( 46,X'S) H ( 462,X'S) H ( 461,X'S) H ( 463,X'S)
RIDE C ( 47,X'S) H ( 472,X'S) H ( 471,X'S) H ( 473,X'S)
RIDE C ( 48,X'S) H ( 481,X'S) H ( 483,X'S) H ( 482,X'S)
RIDE C ( 51,X'S) H ( 511,X'S) H ( 512,X'S)
RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
SAME O(1) C(2) C(3) C(4) C(5) AND
CONT O(1) C(5) C(4) C(3) C(2) AND
CONT O(1) C(6) C(7) C(8) C(9) AND
CONT O(1) C(9) C(8) C(7) C(6)
DELU 0.01 O(1) C(2) C(3) C(4) C(5) AND
CONT O(1) C(5) C(4) C(3) C(2) AND
CONT O(1) C(6) C(7) C(8) C(9) AND
CONT O(1) C(9) C(8) C(7) C(6)
SIMU 0.01 O(1) C(2) C(3) C(4) C(5) AND
CONT O(1) C(5) C(4) C(3) C(2) AND
CONT O(1) C(6) C(7) C(8) C(9) AND
CONT O(1) C(9) C(8) C(7) C(6)
END
;