Neutral, cationic and anionic organonickel and -palladium complexes supported by iminophosphine/phosphinoenaminato ligands.
Santiago, Tomás G; Urbaneja, Carmen; Álvarez, Eleuterio; Ávila, Elena; Palma, Pilar; Cámpora, Juan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 322–335; doi:10.1039/c9dt04062e

data_7701990
_publ_section_title
;
 Neutral, cationic and anionic organonickel and -palladium complexes
 supported by iminophosphine/phosphinoenaminato ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              322
_journal_page_last               335
_journal_paper_doi               10.1039/c9dt04062e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C40 H41 Br N Ni O P'
_chemical_formula_sum            'C40 H41 Br N Ni O P'
_chemical_formula_weight         721.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-11-19 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.9940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9701(2)
_cell_length_b                   14.6823(3)
_cell_length_c                   12.4003(3)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.22
_cell_volume                     1716.37(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24230
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.511
_diffrn_reflns_theta_min         2.160
_exptl_absorpt_coefficient_mu    1.808
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
program SADABS, Bruker (2001). 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       prism
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   -0.004(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         8272
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0236P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.529
_reflns_Friedel_fraction_full    0.666
_reflns_Friedel_fraction_max     0.566
_reflns_number_gt                7647
_reflns_number_total             8272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04062e2.cif
_cod_data_source_block           7b
_cod_depositor_comments
'Adding full bibliography for 7701989--7701993.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7701990
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.661
_shelx_estimated_absorpt_t_max   0.737
_shelx_res_checksum              35811