Nickel Bis-Diphosphine Complexes: Controlling the Binding and Heterolysis of H2
Stolley, Ryan M.; Darmon, Jonathan M.; Das, Parthapratim; Helm, Monte L.; Organometallics 35 (2016) 2965–; doi:10.1021/acs.organomet.6b00486

data_4088847
_publ_section_title
;
 Nickel Bis-Diphosphine Complexes: Controlling the Binding and Heterolysis
 of H2
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2965
_journal_paper_doi               10.1021/acs.organomet.6b00486
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C30 H43 Cl2 N Ni P2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C30.5 H44 Cl3 N Ni P2'
_chemical_formula_weight         651.66
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.646(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.415(3)
_cell_length_b                   10.9653(10)
_cell_length_c                   24.385(2)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.39
_cell_volume                     6833.6(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            65643
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.152
_diffrn_reflns_theta_min         0.797
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0557 before and 0.0451 after correction.
The Ratio of minimum to maximum transmission is 0.8973.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         15119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0412P)^2^+4.7121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12416
_reflns_number_total             15119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00486_si_002.cif
_cod_data_source_block           xprep3
_cod_depositor_comments
;

2020-08-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C61 H88 Cl6 N2 Ni2 P4'
_cod_original_formula_weight         1303.33
_cod_original_formula_moiety         '2(C30 H43 Cl2 N Ni P2), C H2 Cl2'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        6833.7(11)
_cod_database_code               4088847
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.914
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6), C12(H12), C18(H18), C36(H36), C42(H42), C48(H48)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C31(H31A,H31B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
  C61(H61A,H61B)
2.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
  C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
;
_shelx_res_checksum              27823
_shelx_hkl_checksum              60975
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'