An unusual Ni<sub>2</sub>Si<sub>2</sub>P<sub>8</sub> cluster formed by complexation and thermolysis.
Ziegler, Christoph G. P.; Taube, Clemens; Kelly, John A.; Hierlmeier, Gabriele; Uttendorfer, Maria; Weigand, Jan J.; Wolf, Robert; Chemical communications (Cambridge, England) 56 (2020) 14071–14074; doi:10.1039/d0cc05365a

data_7127738
_publ_section_title
;
 An unusual Ni<sub>2</sub>Si<sub>2</sub>P<sub>8</sub> cluster formed by
 complexation and thermolysis.
;
_journal_issue                   90
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14071
_journal_page_last               14074
_journal_paper_doi               10.1039/d0cc05365a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C56 H76 N4 Ni P4 Si'
_chemical_formula_sum            'C56 H76 N4 Ni P4 Si'
_chemical_formula_weight         1015.88
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-24
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-11 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4645(3)
_cell_length_b                   15.4359(3)
_cell_length_c                   42.6490(6)
_cell_measurement_reflns_used    16112
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.4250
_cell_measurement_theta_min      3.9640
_cell_volume                     11497.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     14.00 114.00   1.00   15.00    --   42.29  57.00  30.00  100
  2  \w     30.00  69.00   1.00   60.00    --  106.40 -30.00  90.00   39
  3  \w     33.00 121.00   1.00   60.00    --  106.40-125.00-150.00   88
  4  \w     77.00 158.00   1.00   60.00    --  106.40  61.00  60.00   81
  5  \w     33.00  77.00   1.00   60.00    --  106.40 -45.00 -30.00   44
  6  \w     78.00 158.00   1.00   60.00    --  106.40  30.00 -60.00   80
  7  \w     14.00 114.00   1.00   15.00    --   42.29  57.00-180.00  100
  8  \w    -32.00  67.00   1.00   15.00    --   42.29 -37.00  30.00   99
  9  \w     33.00  77.00   1.00   60.00    --  106.40 -45.00 -90.00   44
 10  \w     30.00  69.00   1.00   60.00    --  106.40 -30.00 150.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0819015000
_diffrn_orient_matrix_UB_12      -0.0131127000
_diffrn_orient_matrix_UB_13      0.0125740000
_diffrn_orient_matrix_UB_21      -0.0318442000
_diffrn_orient_matrix_UB_22      -0.0087955000
_diffrn_orient_matrix_UB_23      0.0335483000
_diffrn_orient_matrix_UB_31      -0.0082028000
_diffrn_orient_matrix_UB_32      -0.0984901000
_diffrn_orient_matrix_UB_33      -0.0046270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            46160
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.993
_diffrn_reflns_theta_min         3.271
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.020
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.37b (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light red'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       block
_exptl_crystal_F_000             4336
_exptl_crystal_recrystallization_method 'from n-hexane'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         11392
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+24.2687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9704
_reflns_number_total             11392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05365a2.cif
_cod_data_source_block           test_op_gauss
_cod_database_code               7127738
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'H76 C56 N4 Ni1 P4 Si1'
_chemical_oxdiff_usercomment     'from n-hexane'
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.564
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
P0 \\sim P006 \\sim P1 \\sim P004 \\sim P005: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N00C \\sim C00O \\sim C00P \\sim C00S \\sim C016 \\sim C019 \\sim C01E \\sim
C01H \\sim C01J \\sim C01M \\sim C01O \\sim C01S \\sim C01T \\sim C01U \\sim
N00D \\sim C1AA \\sim C0 \\sim C1 \\sim C6AA \\sim C9AA \\sim C7 \\sim C34
\\sim C0AA \\sim C2AA \\sim C3 \\sim C9 \\sim C6 \\sim C7AA \\sim C5AA \\sim
C01N \\sim C2 \\sim C017: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
3. Others
 Sof(N00D)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C0)=Sof(C1)=Sof(H1A)=
 Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=
 Sof(H6AC)=Sof(C7AA)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C9AA)=Sof(H9AA)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C34)=Sof(C0AA)=Sof(C2AA)=Sof(H2AA)=Sof(C3)=
 Sof(H3A)=Sof(C9)=Sof(H9A)=Sof(C6)=Sof(C2)=Sof(H2A)=1-FVAR(1)
 Sof(N00C)=Sof(C00O)=Sof(C00P)=Sof(C00S)=Sof(H00S)=Sof(C016)=Sof(C017)=
 Sof(H017)=Sof(C019)=Sof(C01E)=Sof(H01Q)=Sof(C01H)=Sof(H01W)=Sof(C01J)=
 Sof(H01Z)=Sof(C01M)=Sof(H2)=Sof(HE)=Sof(HF)=Sof(C01N)=Sof(H3)=Sof(HG)=Sof(HH)=
 Sof(C01O)=Sof(H4)=Sof(C01S)=Sof(H8)=Sof(HO)=Sof(HP)=Sof(C01T)=Sof(H9)=Sof(HQ)=
 Sof(HR)=Sof(C01U)=Sof(H10)=Sof(HS)=Sof(HT)=FVAR(1)
 Sof(P0)=Sof(P1)=1-FVAR(2)
 Sof(P004)=Sof(P006)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C00Q(H00Q), C00R(H00R), C00T(H00T), C00X(H00X), C00Y(H00Y), C010(H010),
 C01H(H01W), C01O(H4), C1(H1A), C9AA(H9AA)
4.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00G(H00G), C00N(H00N), C00S(H00S), C00U(H00U), C00V(H00V),
 C00W(H00W), C00Z(H00Z), C011(H011), C012(H012), C015(H015), C017(H017),
 C01A(H01J), C01E(H01Q), C01J(H01Z), C2AA(H2AA), C3(H3A), C9(H9A), C2(H2A)
4.c Fitted hexagon refined as free rotating group:
 C34(C0AA,C2AA,C3,C9,C6)
4.d X=CH2 refined with riding coordinates:
 C01F(H01R,H01S)
4.e Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C014(H01D,H01E,H01F), C018(H01G,H01H,H01I), C01C(H01K,
 H01L,H01M), C01D(H01N,H01O,H01P), C01G(H01T,H01U,H01V), C01I(H01X,H01Y,H),
 C01K(H01,HA,HB), C01L(H1,HC,HD), C01M(H2,HE,HF), C01N(H3,HG,HH), C01P(H5,HI,
 HJ), C01Q(H6,HK,HL), C01R(H7,HM,HN), C01S(H8,HO,HP), C01T(H9,HQ,HR), C01U(H10,
 HS,HT), C1AA(H1AA,H1AB,H1AC), C5AA(H5AA,H5AB,H5AC), C6AA(H6AA,H6AB,H6AC),
 C7AA(H7AA,H7AB,H7AC), C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.806