Activation of CO2 by a Heterobimetallic Zr/Co Complex
Jeremy P. Krogman; Bruce M. Foxman; Christine M. Thomas; Journal of the American Chemical Society 133 (2011) 14582–14585; doi:10.1021/ja2071847

data_4106793
_publ_section_title
;
 Activation of CO2 by a Heterobimetallic Zr/Co Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14582
_journal_page_last               14585
_journal_paper_doi               10.1021/ja2071847
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C67 H115 Co1 N3 Na2.00 O9 P3 Zr1'
_chemical_formula_sum            'C67 H115 Co N3 Na2 O9 P3 Zr'
_chemical_formula_weight         1395.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             11-07-10
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 90.003(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3700(5)
_cell_length_b                   24.6113(8)
_cell_length_c                   20.1119(7)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     7112.9(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20407
_diffrn_reflns_theta_full        29.483
_diffrn_reflns_theta_max         30.084
_diffrn_reflns_theta_min         1.308
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       'acicular fragment'
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.648
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.204
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9597
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         20407
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.0043352
_refine_ls_shift/su_mean         0.0002527
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 4.93P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0911
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0911
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                17163
_reflns_number_total             20407
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.48
_oxford_diffrn_Wilson_scale      166.95
_oxford_refine_ls_r_factor_ref   0.0552
_oxford_refine_ls_scale          0.081757(9)
_oxford_reflns_number_all        20407
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'jk_100_0m in P2(1)/n'
_cod_data_source_file            ja2071847_si_002_3.cif
_cod_data_source_block           4
_cod_original_sg_symbol_Hall     '-P 2ybn '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C67 H115 Co1 N3 Na2.00 O9 P3 Zr1'
_cod_database_code               4106793
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT ZR   (    1 ,X'S,U'S)  UNTIL P(3) 
CONT NA(10,X'S,U[ISO]) UNTIL NA(21) 
CONT O(1,X'S,U'S) UNTIL O    (    9 ) 
CONT O    (   40 ,X'S,U[ISO])  UNTIL O   (  51 ) 
CONT N(1,X'S,U'S) UNTIL C(67) 
CONT C(480,X'S,U[ISO]) UNTIL C(511) 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) H   (  53,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) H   (  63,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 111,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   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) H   ( 203,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (  31,X'S) H   ( 311,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   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) H   ( 433,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   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) H   ( 592,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) H   ( 612,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) H   ( 642,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) H   ( 672,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   ( 501,X'S) H   (5011,X'S) H   (5012,X'S) 
RIDE C   ( 500,X'S) H   (5001,X'S) H   (5002,X'S) 
RIDE C   ( 511,X'S) H   (5111,X'S) H   (5112,X'S) 
RIDE C   ( 510,X'S) H   (5101,X'S) H   (5102,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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