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_4088679
_publ_section_title
;
 Zirconium and Hafnium Permethylpentalene Compounds
;
_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 unk
_chemical_compound_source        SYN
_chemical_formula_moiety         'C28 H36 Hf1'
_chemical_formula_sum            'C28 H36 Hf'
_chemical_formula_weight         551.08
_chemical_melting_point          ?
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-22
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.1993(3)
_cell_length_b                   28.0554(5)
_cell_length_c                   18.4489(3)
_cell_measurement_reflns_used    5458
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     8902.2(3)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_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  0.060
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42608
_diffrn_reflns_theta_full        26.949
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         5.203
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.699
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.66
_refine_diff_density_min         -7.16
_refine_ls_extinction_coef       580(30)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9683
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         10122
_refine_ls_number_restraints     553
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.0195052
_refine_ls_shift/su_mean         0.0015718
_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: 
 49.1 75.7 36.9 9.18 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2363
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.2361
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                7166
_reflns_number_total             10125
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.63
_oxford_diffrn_Wilson_scale      400.14
_oxford_refine_ls_r_factor_ref   0.0878
_oxford_refine_ls_scale          0.06891(4)
_oxford_reflns_number_all        10125
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '149fmc12 At 17:46 on 12/12'
_cod_data_source_file            om6b00301_si_002.cif
_cod_data_source_block           1Hf
_cod_depositor_comments
;
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 '_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 2 2 21 '
_cod_original_formula_sum        'C28 H36 Hf1'
_cod_database_code               4088679
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
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   ( 111,X'S) H   ( 112,X'S) H   ( 113,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   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) H   ( 383,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) H   ( 393,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) H   ( 403,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) H   ( 423,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) H   ( 473,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) H   ( 483,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) H   ( 493,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) H   ( 543,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) H   ( 553,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) H   ( 563,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
DIST 0.00,0.01 = MEAN C(1) TO C(2) C(2) TO C(3) 
CONT C(3) TO C(4) C(4) TO C(5) C(5) TO C(6) C(6) TO C(7) 
CONT C(7) TO C(8) 
DIST 0.00,0.01 = MEAN C(15) TO C(16) C(16) TO C(17) 
CONT C(17) TO C(18) C(18) TO C(19) C(19) TO C(20) C(20) TO C(21) 
CONT C(21) TO C(22) 
DIST 0.00,0.01 = MEAN C(29) TO C(30) C(30) TO C(31) 
CONT C(31) TO C(32) C(32) TO C(33) C(33) TO C(34) C(34) TO C(35) 
CONT C(35) TO C(36) 
DIST 0.00,0.01 = MEAN C(43) TO C(44) C(44) TO C(45) 
CONT C(45) TO C(46) 
DIST 0.00,0.01 = MEAN C(50) TO C(51) C(51) TO C(52) 
CONT C(52) TO C(53) 
DIST 0.00,0.01 = MEAN C(1) TO C(9) C(2) TO C(10) 
CONT C(3) TO C(11) C(5) TO C(12) C(6) TO C(13) 
CONT C(7) TO C(14) C(15) TO C(23) C(16) TO C(24) 
CONT C(17) TO C(25) C(19) TO C(26) C(20) TO C(27) 
CONT C(21) TO C(28) C(29) TO C(37) C(30) TO C(38) 
CONT C(31) TO C(39) C(33) TO C(40) C(34) TO C(41) 
CONT C(35) TO C(42) C(43) TO C(47) C(44) TO C(48) 
CONT C(45) TO C(49) C(50) TO C(54) C(51) TO C(55) 
CONT C(52) TO C(56) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.02000 = C(1) TO C(2) 
U(IJ) .0, 0.02000 = C(1) TO C(8) 
U(IJ) .0, 0.04000 = C(1) TO C(9) 
U(IJ) .0, 0.02000 = C(1) TO HF(1) 
U(IJ) .0, 0.02000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(10) 
U(IJ) .0, 0.02000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(3) TO C(11) 
U(IJ) .0, 0.02000 = C(3) TO HF(1) 
U(IJ) .0, 0.02000 = C(4) TO C(5) 
U(IJ) .0, 0.02000 = C(4) TO C(8) 
U(IJ) .0, 0.02000 = C(4) TO HF(1) 
U(IJ) .0, 0.02000 = C(5) TO C(6) 
U(IJ) .0, 0.04000 = C(5) TO C(12) 
U(IJ) .0, 0.02000 = C(5) TO HF(1) 
U(IJ) .0, 0.02000 = C(6) TO C(7) 
U(IJ) .0, 0.04000 = C(6) TO C(13) 
U(IJ) .0, 0.02000 = C(7) TO C(8) 
U(IJ) .0, 0.04000 = C(7) TO C(14) 
U(IJ) .0, 0.02000 = C(7) TO HF(1) 
U(IJ) .0, 0.02000 = C(8) TO HF(1) 
U(IJ) .0, 0.02000 = C(15) TO C(16) 
U(IJ) .0, 0.02000 = C(15) TO C(22) 
U(IJ) .0, 0.04000 = C(15) TO C(23) 
U(IJ) .0, 0.02000 = C(15) TO HF(1) 
U(IJ) .0, 0.02000 = C(16) TO C(17) 
U(IJ) .0, 0.04000 = C(16) TO C(24) 
U(IJ) .0, 0.02000 = C(17) TO C(18) 
U(IJ) .0, 0.04000 = C(17) TO C(25) 
U(IJ) .0, 0.02000 = C(17) TO HF(1) 
U(IJ) .0, 0.02000 = C(18) TO C(19) 
U(IJ) .0, 0.02000 = C(18) TO C(22) 
U(IJ) .0, 0.02000 = C(18) TO HF(1) 
U(IJ) .0, 0.02000 = C(19) TO C(20) 
U(IJ) .0, 0.04000 = C(19) TO C(26) 
U(IJ) .0, 0.02000 = C(19) TO HF(1) 
U(IJ) .0, 0.02000 = C(20) TO C(21) 
U(IJ) .0, 0.04000 = C(20) TO C(27) 
U(IJ) .0, 0.02000 = C(21) TO C(22) 
U(IJ) .0, 0.04000 = C(21) TO C(28) 
U(IJ) .0, 0.02000 = C(21) TO HF(1) 
U(IJ) .0, 0.02000 = C(22) TO HF(1) 
U(IJ) .0, 0.02000 = C(29) TO C(30) 
U(IJ) .0, 0.02000 = C(29) TO C(36) 
U(IJ) .0, 0.04000 = C(29) TO C(37) 
U(IJ) .0, 0.02000 = C(29) TO HF(2) 
U(IJ) .0, 0.02000 = C(30) TO C(31) 
U(IJ) .0, 0.04000 = C(30) TO C(38) 
U(IJ) .0, 0.02000 = C(30) TO HF(2) 
U(IJ) .0, 0.02000 = C(31) TO C(32) 
U(IJ) .0, 0.04000 = C(31) TO C(39) 
U(IJ) .0, 0.02000 = C(32) TO C(33) 
U(IJ) .0, 0.02000 = C(32) TO C(36) 
U(IJ) .0, 0.02000 = C(33) TO C(34) 
U(IJ) .0, 0.04000 = C(33) TO C(40) 
U(IJ) .0, 0.02000 = C(33) TO HF(2) 
U(IJ) .0, 0.02000 = C(34) TO C(35) 
U(IJ) .0, 0.04000 = C(34) TO C(41) 
U(IJ) .0, 0.02000 = C(34) TO HF(2) 
U(IJ) .0, 0.02000 = C(35) TO C(36) 
U(IJ) .0, 0.04000 = C(35) TO C(42) 
U(IJ) .0, 0.02000 = C(35) TO HF(2) 
U(IJ) .0, 0.02000 = C(36) TO HF(2) 
U(IJ) .0, 0.02000 = C(43) TO C(46,3,1,0,0,1) 
U(IJ) .0, 0.02000 = C(43) TO C(44) 
U(IJ) .0, 0.04000 = C(43) TO C(47) 
U(IJ) .0, 0.02000 = C(43) TO HF(3) 
U(IJ) .0, 0.02000 = C(44) TO C(45) 
U(IJ) .0, 0.04000 = C(44) TO C(48) 
U(IJ) .0, 0.02000 = C(45) TO C(46) 
U(IJ) .0, 0.04000 = C(45) TO C(49) 
U(IJ) .0, 0.02000 = C(45) TO HF(3) 
U(IJ) .0, 0.02000 = C(46) TO C(46,3,1,0,0,1) 
U(IJ) .0, 0.02000 = C(46) TO HF(3) 
U(IJ) .0, 0.02000 = C(50) TO C(53,3,1,0,0,1) 
U(IJ) .0, 0.02000 = C(50) TO C(51) 
U(IJ) .0, 0.04000 = C(50) TO C(54) 
U(IJ) .0, 0.02000 = C(50) TO HF(3) 
U(IJ) .0, 0.02000 = C(51) TO C(52) 
U(IJ) .0, 0.04000 = C(51) TO C(55) 
U(IJ) .0, 0.02000 = C(52) TO C(53) 
U(IJ) .0, 0.04000 = C(52) TO C(56) 
U(IJ) .0, 0.02000 = C(52) TO HF(3) 
U(IJ) .0, 0.02000 = C(53) TO C(53,3,1,0,0,1) 
U(IJ) .0, 0.02000 = C(53) TO HF(3) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;