A chromium precursor for the Phillips ethylene trimerization catalyst: (2-ethylhexanoate)2CrOH.
Jeon, Jong Yeob; Park, Dong Sik; Lee, Dong Hwan; Eo, Seong Chan; Park, Seong Yeon; Jeong, Myoung Sun; Kang, Yi Young; Lee, Junseong; Lee, Bun Yeoul; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11004–11012; doi:10.1039/c5dt01203a

data_7035042
_publ_section_title
;
 A chromium precursor for the Phillips ethylene trimerization catalyst:
 (2-ethylhexanoate)2CrOH.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11004
_journal_page_last               11012
_journal_paper_doi               10.1039/c5dt01203a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C28 H51 Al3 Cl4 Cr4 N3'
_chemical_formula_sum            'C28 H51 Al3 Cl4 Cr4 N3'
_chemical_formula_weight         860.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-04-27
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.02.26 svn.r3159 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2015-04-29 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.9370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6198(2)
_cell_length_b                   29.9914(7)
_cell_length_c                   12.3307(3)
_cell_measurement_reflns_used    3526
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      3.41
_cell_volume                     3986.04(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_unetI/netI     0.1042
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27526
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.165
_exptl_absorpt_coefficient_mu    1.418
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.178
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6979
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+21.4707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4278
_reflns_number_total             6979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01203a2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7035040--7035042.cif.'
_cod_database_code               7035042
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C28-H28A = C28-H28B = C28-H28C
 0.9 with sigma of 0.02
 C25-H25A = C25-H25B
 0.9 with sigma of 0.02
 C26-H26A = C26-H26B
 0.9 with sigma of 0.02
 C27-H27A = C27-H27B
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl6) = Uanis(C16)
Uanis(C15) = Uanis(C1B)
Uanis(C1A) = Uanis(Cl2)
Uanis(Al2) = Uanis(Al4) = Uanis(Al5)
Uanis(C16) = Uanis(Cl6) = Uanis(C1C)
Uanis(Cl2) = Uanis(C1A) = Uanis(C1D)
Uanis(C15) = Uanis(C1B) = Uanis(Cl7)
4. Rigid body (RIGU) restrains
 Al2, C15, C16, Cl2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1B, Al4, Cl6, C1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl7, Al5, C1C, C1D
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cl5(0.5) Cl4(0.5) Al2(0.55) C15(0.55) H15A(0.55) H15B(0.55)
 H15C(0.55) C16(0.55) H16A(0.55) H16B(0.55) H16C(0.55) Cl2(0.55) Al4(0.2)
 C1A(0.2) H1AA(0.2) H1AB(0.2) H1AC(0.2) C1B(0.2) H1BA(0.2) H1BB(0.2) H1BC(0.2)
 Cl6(0.2) Al5(0.25) C1C(0.25) H1CA(0.25) H1CB(0.25) H1CC(0.25) C1D(0.25)
 H1DA(0.25) H1DB(0.25) H1DC(0.25) Cl7(0.25)
6.a Free rotating group:
 Al2(C15,C16,Cl2), Al4(C1A,C1B,Cl6), Al5(C1C,C1D,Cl7)
6.b Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C10(H10), C11(H11), C18(H18), C19(H19)
6.c Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,
 H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,H1DC)
6.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'