Synthesis, Structure, and Reactivity of an Anionic Zr-Oxo Relevant to CO2 Reduction by a Zr/Co Heterobimetallic Complex
Jeremy P. Krogman; Mark W. Bezpalko; Bruce M. Foxman; Christine M. Thomas; Inorganic Chemistry 52 (2013) 3022–3031; doi:10.1021/ic302473j

data_4334133
_publ_section_title
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 Synthesis, Structure, and Reactivity of an Anionic Zr-Oxo Relevant to CO2
 Reduction by a Zr/Co Heterobimetallic Complex
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3022
_journal_page_last               3031
_journal_paper_doi               10.1021/ic302473j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C48.95 H84 Co1 I0.05 N3 O1.95 P3 Si1 Zr1'
_chemical_formula_sum            'C48.95 H84 Co I0.05 N3 O1.95 P3 Si Zr'
_chemical_formula_weight         1022.97
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-02-16
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   11.8774(5)
_cell_length_b                   11.8774(5)
_cell_length_c                   129.387(6)
_cell_measurement_reflns_used    6516
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     15807.5(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.078
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       174
_diffrn_reflns_limit_l_min       -161
_diffrn_reflns_number            46605
_diffrn_reflns_theta_full        28.717
_diffrn_reflns_theta_max         28.717
_diffrn_reflns_theta_min         2.005
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       plate
_exptl_crystal_F_000             6513.703
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9701
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.0043073
_refine_ls_shift/su_mean         0.0001521
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +51.92P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0927
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0927
_reflns_limit_h_max              0
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              174
_reflns_limit_l_min              0
_reflns_number_gt                3357
_reflns_number_total             4552
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0575
_oxford_refine_ls_scale          0.0215936(13)
_oxford_reflns_number_all        4552
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'jk_242_2_0m in R-3c'
_cod_data_source_file            ic302473j_si_002_07.cif
_cod_data_source_block           6
_cod_original_cell_volume        15807.6(12)
_cod_original_sg_symbol_Hall     '-R 3 2"c '
_cod_original_sg_symbol_H-M      'R -3 c '
_cod_original_formula_sum        'C48.95 H84 Co1 I0.05 N3 O1.95 P3 Si1 Zr1'
_cod_database_code               4334133
_iucr_refine_instruction_details_constraints
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BLOCK 
CONT SCALE 
CONT ZR   (    1 ,X'S,U'S)  UNTIL CO   (    1 ) 
CONT I    (    1 ,X'S,U[ISO]) 
CONT P    (    1 ,X'S,U'S)  UNTIL O    (    1 ) 
CONT O    (    2 ,X'S,U[ISO]) 
CONT N    (    1 ,X'S,U'S)  UNTIL C    (   16 ) 
CONT C    (   17 ,X'S,U[ISO]) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  13,X'S) H   (  12,X'S) 
RIDE C   (   4,X'S) H   (  43,X'S) H   (  42,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  73,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,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) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 121,X'S) H   ( 123,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 152,X'S) H   ( 151,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 162,X'S) H   ( 161,X'S) H   ( 163,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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