Rapid oxidative hydrogen evolution from a family of square-planar nickel hydride complexes
Ramakrishnan, Srinivasan; Chakraborty, Sumit; Brennessel, William W.; Chidsey, Christopher E. D.; Jones, William D.; Chem. Sci. 7 (2016) 117–; doi:10.1039/C5SC03189C

data_1540459
_publ_section_title
;
 Rapid oxidative hydrogen evolution from a family of square-planar nickel
 hydride complexes
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              117
_journal_paper_doi               10.1039/C5SC03189C
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C23 H41 Cl Ni O3 P2'
_chemical_formula_sum            'C23 H41 Cl Ni O3 P2'
_chemical_formula_weight         521.66
_chemical_name_common            jonsc01
_chemical_name_systematic
; 
 (4-MeO-t-BuPOCOP)NiCl 
;
_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_method           SHELXL-2013
_audit_update_record
;
2015-08-13 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.418(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.485(4)
_cell_length_b                   7.985(2)
_cell_length_c                   23.646(7)
_cell_measurement_reflns_used    4051
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      31.06
_cell_measurement_theta_min      2.70
_cell_volume                     2623.4(13)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            45634
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        32.030
_diffrn_reflns_theta_max         32.181
_diffrn_reflns_theta_min         1.796
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       needle
_exptl_crystal_F_000             1112
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/pentane'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         9223
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0351P)^2^+1.4991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5960
_reflns_number_total             9223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03189c2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 1540459--1540464.cif.'
_cod_original_cell_volume        2623.3(13)
_cod_database_code               1540459
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.891
_shelxl_version_number           2013-4
_shelx_res_checksum              8811