Ni complexes of an alane/tris(phosphine) ligand built around a strongly Lewis acidic tris(<i>N</i>-pyrrolyl)aluminum.
Lai, Qingheng; Cosio, Mario N.; Ozerov, Oleg V.; Chemical communications (Cambridge, England) 56 (2020) 14845–14848; doi:10.1039/d0cc05452f

data_7127469
_publ_section_title
;
 Ni complexes of an alane/tris(phosphine) ligand built around a strongly
 Lewis acidic tris(<i>N</i>-pyrrolyl)aluminum.
;
_journal_issue                   94
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14845
_journal_page_last               14848
_journal_paper_doi               10.1039/d0cc05452f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C30 H51 Al N3 Ni P3'
_chemical_formula_sum            'C30 H51 Al N3 Ni P3'
_chemical_formula_weight         632.33
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-05-13 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.935(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.290(9)
_cell_length_b                   17.502(13)
_cell_length_c                   16.876(13)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.486
_cell_measurement_theta_min      2.305
_cell_volume                     3310(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37302
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         2.327
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1002 before and 0.0464 after correction. The Ratio of minimum to maximum transmission is 0.7772. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+1.8481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6851
_reflns_number_total             7553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05452f2.cif
_cod_data_source_block           p21c_b
_cod_database_code               7127469
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00A(0.025) H00B(0.022) H00C(0.025) H00D(0.027) H00E(0.042)
 H00F(0.042) H00G(0.042) H00H(0.025) H00I(0.028) H00J(0.035) H00K(0.035)
 H00L(0.035) H00M(0.033) H00N(0.043) H00O(0.043) H00P(0.043) H00Q(0.043)
 H00R(0.043) H00S(0.043) H00T(0.034) H00U(0.033) H00V(0.046) H00W(0.046)
 H00X(0.046) H00Y(0.035) H(0.035) HA(0.035) H00Z(0.036) H00(0.043) HB(0.043)
 HC(0.043) H0AA(0.046) HD(0.046) HE(0.046) H1AA(0.037) H2AA(0.042) HF(0.042)
 HG(0.042) H3AA(0.036) H4AA(0.048) HH(0.048) HI(0.048) H5AA(0.035) H6AA(0.048)
 HJ(0.048) HK(0.048) H010(0.043) H01A(0.044) H01B(0.044) H01C(0.044) H012(0.045)
 Fixed X: H00A(0.984393) H00B(0.36752) H00C(0.57999) H00D(0.971707)
 H00E(0.590929) H00F(0.501797) H00G(0.449762) H00H(0.526968) H00I(0.842914)
 H00J(0.487623) H00K(0.365319) H00L(0.486598) H00M(0.684231) H00N(0.331768)
 H00O(0.390437) H00P(0.40197) H00Q(0.563711) H00R(0.485671) H00S(0.624568)
 H00T(1.160537) H00U(0.771177) H00V(0.659965) H00W(0.519152) H00X(0.609998)
 H00Y(0.325402) H(0.272895) HA(0.393896) H00Z(0.479849) H00(1.023793)
 HB(1.086489) HC(1.11519) H0AA(0.79008) HD(0.889814) HE(0.822178) H1AA(0.71451)
 H2AA(0.767319) HF(0.852671) HG(0.903184) H3AA(0.786309) H4AA(0.845512)
 HH(0.822679) HI(0.730646) H5AA(1.051319) H6AA(0.796232) HJ(0.936592)
 HK(0.885909) H010(1.228665) H01A(0.990475) H01B(1.038961) H01C(0.964273)
 H012(0.616277)
 Fixed Y: H00A(0.74856) H00B(0.784105) H00C(0.924101) H00D(0.938765)
 H00E(0.853388) H00F(0.924272) H00G(0.839868) H00H(0.589243) H00I(0.511258)
 H00J(0.640375) H00K(0.656909) H00L(0.695879) H00M(0.459501) H00N(0.890811)
 H00O(0.973465) H00P(0.930051) H00Q(0.686587) H00R(0.618642) H00S(0.625218)
 H00T(0.833907) H00U(0.596412) H00V(0.488888) H00W(0.484227) H00X(0.467548)
 H00Y(0.768187) H(0.697111) HA(0.687962) H00Z(0.892806) H00(0.906176)
 HB(0.836607) HC(0.851871) H0AA(0.764295) HD(0.780217) HE(0.850202)
 H1AA(0.463907) H2AA(0.924081) HF(0.997379) HG(0.91657) H3AA(0.799351)
 H4AA(0.959864) HH(1.024251) HI(0.954944) H5AA(0.697781) H6AA(0.564964)
 HJ(0.549372) HK(0.634294) H010(0.76306) H01A(0.641825) H01B(0.556946)
 H01C(0.576369) H012(0.881858)
 Fixed Z: H00A(0.350234) H00B(0.522978) H00C(0.447852) H00D(0.454926)
 H00E(0.331024) H00F(0.31464) H00G(0.3221) H00H(0.397179) H00I(0.399497)
 H00J(0.527618) H00K(0.563572) H00L(0.602892) H00M(0.518421) H00N(0.430585)
 H00O(0.42407) H00P(0.508109) H00Q(0.306728) H00R(0.263802) H00S(0.254124)
 H00T(0.506242) H00U(0.70941) H00V(0.309268) H00W(0.312839) H00X(0.391264)
 H00Y(0.38508) H(0.429245) HA(0.389576) H00Z(0.635574) H00(0.322044)
 HB(0.281794) HC(0.375648) H0AA(0.284015) HD(0.226248) HE(0.2621)
 H1AA(0.669681) H2AA(0.538043) HF(0.543996) HG(0.577124) H3AA(0.74196)
 H4AA(0.336875) HH(0.400635) HI(0.383693) H5AA(0.676946) H6AA(0.271941)
 HJ(0.28973) HK(0.295797) H010(0.634657) H01A(0.439256) H01B(0.428789)
 H01C(0.501027) H012(0.766309)
;
_shelx_res_checksum              42083
_shelx_hkl_checksum              11703
_olex2_submission_special_instructions 'No special instructions were received'