Zirconium and Hafnium Permethylpentalene Compounds
Chadwick, F. Mark; Cooper, Robert T.; O’Hare, Dermot; Organometallics 35 (2016) 2092–; doi:10.1021/acs.organomet.6b00301

data_4088685
_publ_section_title
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 Zirconium and Hafnium Permethylpentalene Compounds
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_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2092
_journal_paper_doi               10.1021/acs.organomet.6b00301
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_compound_source        SYN
_chemical_formula_moiety         'C35 H37 Hf, C16 H32 Li O8'
_chemical_formula_sum            'C51 H69 Hf Li O8'
_chemical_formula_weight         995.53
_chemical_melting_point          ?
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2016-03-22
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 94.0623(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.00900(10)
_cell_length_b                   21.7049(2)
_cell_length_c                   22.2006(2)
_cell_measurement_reflns_used    29504
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     4810.84(8)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55025
_diffrn_reflns_theta_full        76.306
_diffrn_reflns_theta_max         76.306
_diffrn_reflns_theta_min         3.992
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.412
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.26
_refine_diff_density_min         -0.65
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.523(19)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9593
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         5017
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.0023581
_refine_ls_shift/su_mean         0.0001765
_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: 
 0.351E+04 0.398E+04 0.440E+04 0.140E+04 0.122E+04 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0677
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0677
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                4929
_reflns_number_total             5037
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.38
_oxford_diffrn_Wilson_scale      0.18
_oxford_refine_ls_r_factor_ref   0.0265
_oxford_refine_ls_scale          2.496(14)
_oxford_reflns_number_all        5017
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'C:\Users\ASWGroup\Contacts\Deskt At 13:33 on'
_cod_data_source_file            om6b00301_si_002.cif
_cod_data_source_block           5aHf
_cod_depositor_comments
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The following automatic conversions were performed:

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

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C 1 c 1 '
_cod_original_formula_sum        'C51 H69 Hf1 Li1 O8'
_cod_database_code               4088685
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 113,X'S) H   ( 112,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) 
RIDE C   ( 510,X'S) H   (5101,X'S) H   (5102,X'S) 
RIDE C   ( 511,X'S) H   (5111,X'S) H   (5112,X'S) 
RIDE C   ( 480,X'S) H   (4801,X'S) H   (4802,X'S) 
RIDE C   ( 481,X'S) H   (4811,X'S) H   (4812,X'S) 
RIDE C   ( 490,X'S) H   (4901,X'S) H   (4902,X'S) 
RIDE C   ( 491,X'S) H   (4911,X'S) H   (4912,X'S) 
RIDE C   ( 500,X'S) H   (5001,X'S) H   (5002,X'S) 
RIDE C   ( 501,X'S) H   (5011,X'S) H   (5012,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
NO 
DIST 1.46,.0002 =  C(480) TO C(491) 
DIST 1.46,.0002 =   C(501) TO C(510) 
DIST 1.46,.0002 =  C(481) TO C(490) 
DIST 1.46,.0002 =  C(500) TO C(511) 
DIST 1.42,.0002 =  O(71) TO C(480) 
DIST 1.42,.0002 =  O(81) TO C(491) 
DIST 1.42,.0002 =  O(81) TO C(501) 
DIST 1.42,.0002 =  O(71) TO C(510) 
DIST 1.42,.0002 =  O(70) TO C(481) 
DIST 1.42,.0002 =  O(80) TO C(490) 
DIST 1.42,.0002 =  O(80) TO C(500) 
DIST 1.42,.0002 = O(70) TO C(511) 
U(IJ) 0.0, .0002 =  C(480) TO C(491) 
U(IJ) 0.0, .0002 =   C(501) TO C(510) 
U(IJ) 0.0, .0002 = C(481) TO C(490) 
U(IJ) 0.0, .0002 = C(500) TO C(511) 
U(IJ) 0.0, .0002 =  O(71) TO C(480) 
U(IJ) 0.0, .0002=  O(81) TO C(491) 
U(IJ) 0.0, .0002=  O(81) TO C(501) 
U(IJ) 0.0, .0002 =  O(71) TO C(510) 
U(IJ) 0.0, .0002=  O(70) TO C(481) 
U(IJ) 0.0, .0002=  O(80) TO C(490) 
U(IJ) 0.0, .0002=  O(80) TO C(500) 
U(IJ) 0.0, .0002= O(70) TO C(511) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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