Aminophobanes: hydrolytic stability, tautomerism and application in Cr-catalysed ethene oligomerisation.
Haddow, Mairi F.; Jaltai, Judit; Hanton, Martin; Pringle, Paul G.; Rush, Laura E.; Sparkes, Hazel A.; Woodall, Christopher H.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2294–2307; doi:10.1039/c5dt04394h

data_7037946
_publ_section_title
;
 Aminophobanes: hydrolytic stability, tautomerism and application in
 Cr-catalysed ethene oligomerisation.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2294
_journal_page_last               2307
_journal_paper_doi               10.1039/c5dt04394h
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ukn
_chemical_formula_moiety         'C27 H31 Cr N O4 P2'
_chemical_formula_sum            'C27 H31 Cr N O4 P2'
_chemical_formula_weight         547.47
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_audit_update_record
;
2015-10-26 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.05490(10)
_cell_length_b                   10.8831(2)
_cell_length_c                   23.6863(4)
_cell_measurement_reflns_used    30546
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.516
_cell_measurement_theta_min      3.188
_cell_volume                     2591.96(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 9.091
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30546
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.516
_diffrn_reflns_theta_min         3.188
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0918 before and 0.0806 after correction. The Ratio of minimum to maximum transmission is 0.6707. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 2125 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.020(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0325P)^2^+0.5084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.767
_reflns_friedel_fraction_full    0.998
_reflns_friedel_fraction_max     0.992
_reflns_number_gt                5301
_reflns_number_total             5929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04394h1.cif
_cod_data_source_block           jj82
_cod_depositor_comments
'Adding full bibliography for 7037938--7037946.cif.'
_cod_database_code               7037946
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.027) H4(0.03) H5(0.029) H6(0.023) H8(0.026) H9(0.035)
 H10(0.033) H11(0.026) H13A(0.034) H13B(0.034) H13C(0.034) H14A(0.034)
 H14B(0.034) H15A(0.026) H15B(0.026) H16(0.021) H17(0.02) H18A(0.026)
 H18B(0.026) H19A(0.027) H19B(0.027) H20A(0.03) H20B(0.03) H25A(0.027)
 H25B(0.027) H26A(0.034) H26B(0.034) H26C(0.034) H27A(0.038) H27B(0.038)
 H27C(0.038)
 Fixed X: H3(0.7168) H4(0.6319) H5(0.4075) H6(0.2719) H8(0.365) H9(0.4019)
 H10(0.374) H11(0.3116) H13A(0.4616) H13B(0.5241) H13C(0.4943) H14A(0.3429)
 H14B(0.1849) H15A(0.2253) H15B(0.3339) H16(0.194) H17(0.1426) H18A(0.0135)
 H18B(-0.0323) H19A(-0.0643) H19B(-0.0252) H20A(-0.1328) H20B(-0.0008)
 H25A(0.3584) H25B(0.2504) H26A(0.5744) H26B(0.5879) H26C(0.7057) H27A(0.1809)
 H27B(0.256) H27C(0.3344)
 Fixed Y: H3(1.1654) H4(1.2671) H5(1.2467) H6(1.1186) H8(0.7889) H9(0.7951)
 H10(0.9796) H11(1.1555) H13A(0.6951) H13B(0.8273) H13C(0.734) H14A(0.4112)
 H14B(0.4044) H15A(0.4684) H15B(0.5663) H16(0.7043) H17(0.6691) H18A(0.5656)
 H18B(0.6897) H19A(0.6578) H19B(0.5222) H20A(0.536) H20B(0.4547) H25A(0.5759)
 H25B(0.4906) H26A(1.0686) H26B(0.9379) H26C(1.0364) H27A(1.1882) H27B(1.2653)
 H27C(1.2232)
 Fixed Z: H3(0.405) H4(0.4823) H5(0.5071) H6(0.4535) H8(0.2777) H9(0.1803)
 H10(0.1311) H11(0.1793) H13A(0.4163) H13B(0.4033) H13C(0.3526) H14A(0.3987)
 H14B(0.4041) H15A(0.3139) H15B(0.3338) H16(0.4894) H17(0.3041) H18A(0.4976)
 H18B(0.4674) H19A(0.3455) H19B(0.326) H20A(0.4176) H20B(0.4161) H25A(0.4566)
 H25B(0.4865) H26A(0.2947) H26B(0.3252) H26C(0.3299) H27A(0.3068) H27B(0.2589)
 H27C(0.3144)
;