3d Early Transition Metal Complexes Supported by a New Sterically Demanding Aryloxide Ligand
Keith Searles; Ba L. Tran; Maren Pink; Chun-Hsing Chen; Daniel J. Mindiola; Inorganic Chemistry 52 (2013) 11126–11135; doi:10.1021/ic401363p

data_4336188
_publ_section_title
;
 3d Early Transition Metal Complexes Supported by a New Sterically
 Demanding Aryloxide Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11126
_journal_page_last               11135
_journal_paper_doi               10.1021/ic401363p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C94 H98 Cl1 Cr1 O4'
_chemical_formula_sum            'C94 H98 Cl Cr O4'
_chemical_formula_weight         1379.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-04-16
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 105.8380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4411(6)
_cell_length_b                   16.1932(6)
_cell_length_c                   26.2278(9)
_cell_measurement_reflns_used    9015
_cell_measurement_temperature    100
_cell_measurement_theta_max      19
_cell_measurement_theta_min      2
_cell_volume                     7534.8(5)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      '0.5 degree frames measured for 0.3s each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Si 1 1 1 and 3 1 1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.087
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            163228
_diffrn_reflns_theta_full        18.844
_diffrn_reflns_theta_max         19.228
_diffrn_reflns_theta_min         0.869
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       plate
_exptl_crystal_F_000             2940.000
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.94
_refine_diff_density_min         -1.17
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         31663
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.0166845
_refine_ls_shift/su_mean         0.0002565
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 3.95P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1556
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1539
_reflns_limit_h_max              28
_reflns_limit_h_min              -29
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                20234
_reflns_number_total             31710
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.39
_oxford_diffrn_Wilson_scale      38.56
_oxford_refine_ls_r_factor_ref   0.1060
_oxford_refine_ls_scale          0.16583(5)
_oxford_reflns_number_all        31673
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'CMC0949_0m in P2(1)/c'
_cod_data_source_file            ic401363p_si_004.cif
_cod_data_source_block           CMC0949
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C94 H98 Cl1 Cr1 O4'
_cod_database_code               4336188
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT CR   (    1 ,X'S,U'S)  UNTIL C    (   42 ) 
CONT C    (   43 ,X'S,U[ISO])  UNTIL C    (   46 ) 
CONT C    (   47 ,X'S,U'S)  UNTIL C    (  941 ) 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
SUMFIX PART(1003,OCC) AND PART(1004,OCC) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
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) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,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   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,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) 
RIDE C   (  30,X'S) H   ( 301,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) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) H   ( 443,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   ( 461,X'S) H   ( 462,X'S) H   ( 463,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) H   ( 742,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) H   ( 752,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) H   ( 772,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) H   ( 782,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) H   ( 792,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) H   ( 802,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) H   ( 872,X'S) H   ( 873,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) H   ( 892,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) H   ( 942,X'S) H   ( 943,X'S) 
RIDE C   ( 441,X'S) H   (4411,X'S) H   (4412,X'S) H   (4413,X'S) 
RIDE C   ( 451,X'S) H   (4511,X'S) H   (4512,X'S) H   (4513,X'S) 
RIDE C   ( 461,X'S) H   (4611,X'S) H   (4612,X'S) H   (4613,X'S) 
RIDE C   ( 901,X'S) H   (9011,X'S) 
RIDE C   ( 911,X'S) H   (9111,X'S) 
RIDE C   ( 921,X'S) H   (9211,X'S) 
RIDE C   ( 931,X'S) H   (9311,X'S) 
RIDE C   ( 941,X'S) H   (9411,X'S) H   (9412,X'S) H   (9413,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
SAME 0.1, 0.01 
CONT C(88) C(89) C(90) C(91) C(92) C(93) C(94) AND 
CONT C(88) C(93) C(92) C(91) C(90) C(89) C(94) AND 
CONT C(881) C(931) C(921) C(911) C(901) C(89) C(941) AND 
CONT C(881) C(89) C(901) C(911) C(921) C(931) C(941) 
SAME 0.1, 0.01 
CONT C(43) C(40) C(44) C(45) C(46) AND 
CONT C(43) C(40) C(46) C(45) C(44) AND 
CONT C(431) C(40) C(441) C(451) C(461) AND 
CONT C(431) C(40) C(461) C(451) C(441) 
END                                                                             
;