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_7037944
_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_formula_moiety         'C23 H32 N P2, Cl'
_chemical_formula_sum            'C23 H32 Cl N P2'
_chemical_formula_weight         419.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90.00
_cell_angle_beta                 100.569(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8271(8)
_cell_length_b                   8.5130(4)
_cell_length_c                   15.6725(8)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.46
_cell_volume                     2206.98(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19574
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.23
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5066
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0330P)^2^+1.2232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                4682
_reflns_number_total             5066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04394h1.cif
_cod_data_source_block           jj353
_cod_depositor_comments
'Adding full bibliography for 7037938--7037946.cif.'
_cod_database_code               7037944
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1N(0.017) H1A(0.019) H2A(0.025) H2B(0.025) H3A(0.028) H3B(0.028)
 H4A(0.022) H4B(0.022) H5(0.017) H6A(0.022) H6B(0.022) H7A(0.027) H7B(0.027)
 H8A(0.024) H8B(0.024) H9(0.019) H10A(0.033) H10B(0.033) H10C(0.033)
 H11A(0.034) H11B(0.034) H11C(0.034) H13(0.021) H14(0.024) H15(0.024)
 H16(0.023) H17(0.02) H19(0.023) H20(0.029) H21(0.027) H22(0.023) H23(0.02)
 Fixed X: H1A(0.1503) H2A(0.2126) H2B(0.1203) H3A(0.1772) H3B(0.0912)
 H4A(0.1614) H4B(0.2422) H5(0.1946) H6A(0.0696) H6B(0.0535) H7A(0.0103) H7B(-
 0.0355) H8A(0.0129) H8B(0.0421) H9(0.1802) H10A(0.0939) H10B(0.0957)
 H10C(0.0529) H11A(0.2994) H11B(0.2433) H11C(0.2484) H13(0.2891) H14(0.3419)
 H15(0.453) H16(0.5116) H17(0.4556) H19(0.4205) H20(0.4599) H21(0.425)
 H22(0.3579) H23(0.3231)
 Fixed Y: H1A(1.2611) H2A(1.3076) H2B(1.3587) H3A(1.2201) H3B(1.1586)
 H4A(0.9369) H4B(1.0018) H5(0.8004) H6A(0.7973) H6B(0.8017) H7A(1.0579)
 H7B(0.9694) H8A(1.2249) H8B(1.0892) H9(1.0983) H10A(0.8173) H10B(0.9717)
 H10C(0.9761) H11A(0.9599) H11B(0.9622) H11C(0.8073) H13(1.3152) H14(1.3914)
 H15(1.2591) H16(1.0501) H17(0.9655) H19(0.9587) H20(0.7091) H21(0.4874)
 H22(0.5151) H23(0.7646)
 Fixed Z: H1A(0.297) H2A(0.4396) H2B(0.4309) H3A(0.5637) H3B(0.5151)
 H4A(0.558) H4B(0.5311) H5(0.4357) H6A(0.3416) H6B(0.4388) H7A(0.4259)
 H7B(0.3412) H8A(0.3113) H8B(0.254) H9(0.1683) H10A(0.1072) H10B(0.0494)
 H10C(0.1325) H11A(0.1604) H11B(0.0661) H11C(0.1247) H13(0.2686) H14(0.1469)
 H15(0.1108) H16(0.1968) H17(0.3147) H19(0.5536) H20(0.608) H21(0.5215)
 H22(0.3782) H23(0.3212)
;