Synthesis of a mononuclear, non-square-planar chromium(ii) bis(alkoxide) complex and its reactivity toward organic carbonyls and CO2.
Yousif, Maryam; Cabelof, Alyssa C.; Martin, Philip D.; Lord, Richard L.; Groysman, Stanislav; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9794–9804; doi:10.1039/c6dt00279j

data_7038947
_publ_section_title
;
 Synthesis of a mononuclear, non-square-planar chromium(ii) bis(alkoxide)
 complex and its reactivity toward organic carbonyls and CO2.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9794
_journal_page_last               9804
_journal_paper_doi               10.1039/c6dt00279j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C74 H98 Cr O12'
_chemical_formula_weight         1231.52
_chemical_name_systematic        'compound 8'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-04 deposited with the CCDC.
2016-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                78.612(6)
_cell_angle_beta                 85.689(6)
_cell_angle_gamma                76.473(5)
_cell_formula_units_Z            4
_cell_length_a                   13.8974(15)
_cell_length_b                   16.8586(18)
_cell_length_c                   28.648(4)
_cell_measurement_reflns_used    15428
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      0.73
_cell_volume                     6394.3(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            160125
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         0.73
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.9761
_exptl_absorpt_correction_T_min  0.9530
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2648
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.328
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1466
_refine_ls_number_reflns         16399
_refine_ls_number_restraints     1443
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.2060
_refine_ls_R_factor_gt           0.1550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+163.1876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3732
_refine_ls_wR_factor_ref         0.4095
_reflns_number_gt                10855
_reflns_number_total             16399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00279j2.cif
_cod_data_source_block           compound_8
_cod_depositor_comments          'Adding full bibliography for 7038947.cif.'
_cod_original_cell_volume        6394.3(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7038947
_solvent_exptl_crystal_recrystallization_method THF