Reversible nickel-metallacycle formation with a phosphinimine-based pincer ligand.
Xing, Xiujing; Zhang, Shaoguang; Thierer, Laura M.; Gau, Michael R.; Carroll, Patrick J.; Tomson, Neil C.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7796–7806; doi:10.1039/d0dt01118e

data_7704491
_publ_section_title
;
 Reversible nickel-metallacycle formation with a phosphinimine-based
 pincer ligand.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7796
_journal_page_last               7806
_journal_paper_doi               10.1039/d0dt01118e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43.4 H38.5 Cl0.1 N3 Ni O0.9 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C51.4 H54.5 Cl0.1 N3 Ni O2.9 P2'
_chemical_formula_weight         884.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-04-22 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                100.184(2)
_cell_angle_beta                 93.978(2)
_cell_angle_gamma                102.322(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5572(6)
_cell_length_b                   11.7407(6)
_cell_length_c                   16.9501(8)
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.562
_cell_measurement_theta_min      3.214
_cell_volume                     2197.81(19)
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       'Bruker APEX3 v2016.1-0'
_computing_data_reduction        'SAINT V8.38A (2016)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58237
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         3.214
_diffrn_source                   'sealed tube'
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_exptl_absorpt_correction_T_min  0.7156
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_exptl_absorpt_process_details   'SADABS v2016/2'
_exptl_crystal_colour            'dark brown'
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.465
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_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0280P)^2^+2.6989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                8500
_reflns_number_total             10118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01118e2.cif
_cod_data_source_block           3366
_cod_depositor_comments
'Adding full bibliography for 7704491--7704494.cif.'
_cod_original_formula_sum        'C51.40 H54.50 Cl0.10 N3 Ni O2.90 P2'
_cod_database_code               7704491
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.871