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_4088680
_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_compound_source        SYN
_chemical_formula_moiety         'C28 H36 Zr1'
_chemical_formula_sum            'C28 H36 Zr'
_chemical_formula_weight         463.81
_chemical_melting_point          ?
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                90.0147(8)
_cell_angle_beta                 89.9752(8)
_cell_angle_gamma                117.3070(9)
_cell_formula_units_Z            8
_cell_length_a                   16.5220(3)
_cell_length_b                   16.5205(3)
_cell_length_c                   18.4637(4)
_cell_measurement_reflns_used    18781
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4478.08(15)
_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_pressure         100
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_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  0.044
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34489
_diffrn_reflns_theta_full        25.860
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         5.189
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.61
_refine_diff_density_min         -2.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0521
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         20209
_refine_ls_number_restraints     1008
_refine_ls_R_factor_all          0.1816
_refine_ls_R_factor_gt           0.1315
_refine_ls_shift/su_max          0.0091017
_refine_ls_shift/su_mean         0.0009604
_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: 
 16.2 16.3 4.43 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1557
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1556
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                12191
_reflns_number_total             20219
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.88
_oxford_diffrn_Wilson_scale      57.80
_oxford_refine_ls_r_factor_ref   0.1815
_oxford_refine_ls_scale          0.18291(7)
_oxford_reflns_number_all        20219
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '144fmc12 At 15:23 on 4/10'
_cod_data_source_file            om6b00301_si_002.cif
_cod_data_source_block           1Zr
_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 '_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      'P -1 '
_cod_original_formula_sum        'C28 H36 Zr1'
_cod_database_code               4088680
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  93,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,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   ( 122,X'S) H   ( 123,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) 
RIDE C   (  22,X'S) H   ( 223,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 233,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 253,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 263,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 272,X'S) H   ( 271,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 283,X'S) H   ( 281,X'S) 
RIDE C   (  37,X'S) H   ( 373,X'S) H   ( 371,X'S) H   ( 372,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   ( 392,X'S) H   ( 393,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 413,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 422,X'S) H   ( 421,X'S) H   ( 423,X'S) 
RIDE C   (  51,X'S) H   ( 512,X'S) H   ( 513,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 523,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) H   ( 533,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 543,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 553,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 563,X'S) H   ( 562,X'S) 
RIDE C   (  65,X'S) H   ( 652,X'S) H   ( 651,X'S) H   ( 653,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 663,X'S) H   ( 662,X'S) 
RIDE C   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) H   ( 673,X'S) 
RIDE C   (  68,X'S) H   ( 682,X'S) H   ( 683,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 693,X'S) H   ( 691,X'S) H   ( 692,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) H   ( 703,X'S) H   ( 702,X'S) 
RIDE C   (  79,X'S) H   ( 792,X'S) H   ( 791,X'S) H   ( 793,X'S) 
RIDE C   (  80,X'S) H   ( 803,X'S) H   ( 801,X'S) H   ( 802,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) H   ( 813,X'S) H   ( 812,X'S) 
RIDE C   (  82,X'S) H   ( 822,X'S) H   ( 821,X'S) H   ( 823,X'S) 
RIDE C   (  83,X'S) H   ( 832,X'S) H   ( 833,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 843,X'S) H   ( 841,X'S) H   ( 842,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) H   ( 932,X'S) H   ( 933,X'S) 
RIDE C   (  94,X'S) H   ( 942,X'S) H   ( 943,X'S) H   ( 941,X'S) 
RIDE C   (  95,X'S) H   ( 953,X'S) H   ( 951,X'S) H   ( 952,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) H   ( 963,X'S) H   ( 962,X'S) 
RIDE C   (  97,X'S) H   ( 972,X'S) H   ( 971,X'S) H   ( 973,X'S) 
RIDE C   (  98,X'S) H   ( 982,X'S) H   ( 983,X'S) H   ( 981,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) H   (1073,X'S) H   (1072,X'S) 
RIDE C   ( 108,X'S) H   (1082,X'S) H   (1081,X'S) H   (1083,X'S) 
RIDE C   ( 109,X'S) H   (1092,X'S) H   (1093,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1103,X'S) H   (1101,X'S) H   (1102,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) H   (1113,X'S) H   (1112,X'S) 
RIDE C   ( 112,X'S) H   (1122,X'S) H   (1121,X'S) H   (1123,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
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 ZR(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 ZR(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 ZR(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 ZR(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, 0.01000 = C(7) TO C(23) 
U(IJ) .0, 0.02000 = C(7) TO ZR(1) 
U(IJ) .0, 0.02000 = C(8) TO ZR(1) 
U(IJ) .0, 0.02000 = C(14) TO C(15) 
U(IJ) .0, 0.02000 = C(14) TO C(21) 
U(IJ) .0, 0.04000 = C(14) TO C(22) 
U(IJ) .0, 0.02000 = C(14) TO ZR(1) 
U(IJ) .0, 0.02000 = C(15) TO C(16) 
U(IJ) .0, 0.04000 = C(15) TO C(24) 
U(IJ) .0, 0.02000 = C(16) TO C(17) 
U(IJ) .0, 0.01000 = C(16) TO C(25) 
U(IJ) .0, 0.02000 = C(16) TO ZR(1) 
U(IJ) .0, 0.02000 = C(17) TO C(18) 
U(IJ) .0, 0.02000 = C(17) TO C(21) 
U(IJ) .0, 0.02000 = C(17) TO ZR(1) 
U(IJ) .0, 0.02000 = C(18) TO C(19) 
U(IJ) .0, 0.04000 = C(18) TO C(26) 
U(IJ) .0, 0.02000 = C(18) TO ZR(1) 
U(IJ) .0, 0.02000 = C(19) TO C(20) 
U(IJ) .0, 0.04000 = C(19) TO C(27) 
U(IJ) .0, 0.02000 = C(20) TO C(21) 
U(IJ) .0, 0.04000 = C(20) TO C(28) 
U(IJ) .0, 0.02000 = C(20) TO ZR(1) 
U(IJ) .0, 0.02000 = C(21) TO ZR(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 ZR(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(31) TO C(32) 
U(IJ) .0, 0.04000 = C(31) TO C(39) 
U(IJ) .0, 0.02000 = C(31) TO ZR(2) 
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(32) TO ZR(2) 
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 ZR(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(35) TO C(36) 
U(IJ) .0, 0.04000 = C(35) TO C(42) 
U(IJ) .0, 0.02000 = C(35) TO ZR(2) 
U(IJ) .0, 0.02000 = C(36) TO ZR(2) 
U(IJ) .0, 0.02000 = C(43) TO C(44) 
U(IJ) .0, 0.02000 = C(43) TO C(47) 
U(IJ) .0, 0.02000 = C(43) TO C(50) 
U(IJ) .0, 0.02000 = C(43) TO ZR(2) 
U(IJ) .0, 0.02000 = C(44) TO C(45) 
U(IJ) .0, 0.04000 = C(44) TO C(51) 
U(IJ) .0, 0.02000 = C(44) TO ZR(2) 
U(IJ) .0, 0.02000 = C(45) TO C(46) 
U(IJ) .0, 0.04000 = C(45) TO C(52) 
U(IJ) .0, 0.02000 = C(46) TO C(47) 
U(IJ) .0, 0.04000 = C(46) TO C(53) 
U(IJ) .0, 0.02000 = C(46) TO ZR(2) 
U(IJ) .0, 0.02000 = C(47) TO C(48) 
U(IJ) .0, 0.02000 = C(47) TO ZR(2) 
U(IJ) .0, 0.02000 = C(48) TO C(49) 
U(IJ) .0, 0.04000 = C(48) TO C(54) 
U(IJ) .0, 0.02000 = C(48) TO ZR(2) 
U(IJ) .0, 0.02000 = C(49) TO C(50) 
U(IJ) .0, 0.04000 = C(49) TO C(55) 
U(IJ) .0, 0.04000 = C(50) TO C(56) 
U(IJ) .0, 0.02000 = C(50) TO ZR(2) 
U(IJ) .0, 0.02000 = C(57) TO C(58) 
U(IJ) .0, 0.02000 = C(57) TO C(64) 
U(IJ) .0, 0.01000 = C(57) TO C(65) 
U(IJ) .0, 0.02000 = C(57) TO ZR(3) 
U(IJ) .0, 0.02000 = C(58) TO C(59) 
U(IJ) .0, 0.04000 = C(58) TO C(66) 
U(IJ) .0, 0.02000 = C(59) TO C(60) 
U(IJ) .0, 0.04000 = C(59) TO C(67) 
U(IJ) .0, 0.02000 = C(59) TO ZR(3) 
U(IJ) .0, 0.02000 = C(60) TO C(61) 
U(IJ) .0, 0.02000 = C(60) TO C(64) 
U(IJ) .0, 0.02000 = C(60) TO ZR(3) 
U(IJ) .0, 0.02000 = C(61) TO C(62) 
U(IJ) .0, 0.04000 = C(61) TO C(68) 
U(IJ) .0, 0.02000 = C(61) TO ZR(3) 
U(IJ) .0, 0.02000 = C(62) TO C(63) 
U(IJ) .0, 0.04000 = C(62) TO C(69) 
U(IJ) .0, 0.02000 = C(63) TO C(64) 
U(IJ) .0, 0.04000 = C(63) TO C(70) 
U(IJ) .0, 0.02000 = C(63) TO ZR(3) 
U(IJ) .0, 0.02000 = C(64) TO ZR(3) 
U(IJ) .0, 0.02000 = C(71) TO C(72) 
U(IJ) .0, 0.02000 = C(71) TO C(78) 
U(IJ) .0, 0.01000 = C(71) TO C(79) 
U(IJ) .0, 0.02000 = C(71) TO ZR(3) 
U(IJ) .0, 0.02000 = C(72) TO C(73) 
U(IJ) .0, 0.04000 = C(72) TO C(80) 
U(IJ) .0, 0.02000 = C(73) TO C(74) 
U(IJ) .0, 0.04000 = C(73) TO C(81) 
U(IJ) .0, 0.02000 = C(73) TO ZR(3) 
U(IJ) .0, 0.02000 = C(74) TO C(75) 
U(IJ) .0, 0.02000 = C(74) TO C(78) 
U(IJ) .0, 0.02000 = C(74) TO ZR(3) 
U(IJ) .0, 0.02000 = C(75) TO C(76) 
U(IJ) .0, 0.04000 = C(75) TO C(82) 
U(IJ) .0, 0.02000 = C(75) TO ZR(3) 
U(IJ) .0, 0.02000 = C(76) TO C(77) 
U(IJ) .0, 0.04000 = C(76) TO C(83) 
U(IJ) .0, 0.02000 = C(77) TO C(78) 
U(IJ) .0, 0.04000 = C(77) TO C(84) 
U(IJ) .0, 0.02000 = C(77) TO ZR(3) 
U(IJ) .0, 0.02000 = C(78) TO ZR(3) 
U(IJ) .0, 0.02000 = C(85) TO C(86) 
U(IJ) .0, 0.02000 = C(85) TO C(92) 
U(IJ) .0, 0.04000 = C(85) TO C(93) 
U(IJ) .0, 0.02000 = C(85) TO ZR(4) 
U(IJ) .0, 0.02000 = C(86) TO C(87) 
U(IJ) .0, 0.04000 = C(86) TO C(94) 
U(IJ) .0, 0.02000 = C(87) TO C(88) 
U(IJ) .0, 0.04000 = C(87) TO C(95) 
U(IJ) .0, 0.02000 = C(87) TO ZR(4) 
U(IJ) .0, 0.02000 = C(88) TO C(89) 
U(IJ) .0, 0.02000 = C(88) TO C(92) 
U(IJ) .0, 0.02000 = C(88) TO ZR(4) 
U(IJ) .0, 0.02000 = C(89) TO C(90) 
U(IJ) .0, 0.04000 = C(89) TO C(96) 
U(IJ) .0, 0.02000 = C(89) TO ZR(4) 
U(IJ) .0, 0.02000 = C(90) TO C(91) 
U(IJ) .0, 0.04000 = C(90) TO C(97) 
U(IJ) .0, 0.02000 = C(91) TO C(92) 
U(IJ) .0, 0.04000 = C(91) TO C(98) 
U(IJ) .0, 0.02000 = C(91) TO ZR(4) 
U(IJ) .0, 0.02000 = C(92) TO ZR(4) 
U(IJ) .0, 0.02000 = C(99) TO C(100) 
U(IJ) .0, 0.02000 = C(99) TO C(106) 
U(IJ) .0, 0.04000 = C(99) TO C(107) 
U(IJ) .0, 0.02000 = C(99) TO ZR(4) 
U(IJ) .0, 0.02000 = C(100) TO C(101) 
U(IJ) .0, 0.04000 = C(100) TO C(108) 
U(IJ) .0, 0.02000 = C(101) TO C(102) 
U(IJ) .0, 0.04000 = C(101) TO C(109) 
U(IJ) .0, 0.02000 = C(101) TO ZR(4) 
U(IJ) .0, 0.02000 = C(102) TO C(103) 
U(IJ) .0, 0.02000 = C(102) TO C(106) 
U(IJ) .0, 0.02000 = C(102) TO ZR(4) 
U(IJ) .0, 0.02000 = C(103) TO C(104) 
U(IJ) .0, 0.04000 = C(103) TO C(110) 
U(IJ) .0, 0.02000 = C(103) TO ZR(4) 
U(IJ) .0, 0.02000 = C(104) TO C(105) 
U(IJ) .0, 0.04000 = C(104) TO C(111) 
U(IJ) .0, 0.02000 = C(105) TO C(106) 
U(IJ) .0, 0.04000 = C(105) TO C(112) 
U(IJ) .0, 0.02000 = C(105) TO ZR(4) 
U(IJ) .0, 0.02000 = C(106) TO ZR(4) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;