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_7127736
_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         'C85 H116 N6 Ni P8 Si2, C6 H14'
_chemical_formula_sum            'C91 H130 N6 Ni P8 Si2'
_chemical_formula_weight         1670.65
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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     dual
_audit_creation_date             2019-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-11 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.741(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6231(4)
_cell_length_b                   13.31130(10)
_cell_length_c                   30.4842(5)
_cell_measurement_reflns_used    24574
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.1880
_cell_measurement_theta_min      3.8170
_cell_volume                     9226.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 1.000
_diffrn_measured_fraction_theta_max 0.982
_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    -20.00  83.00   1.00    7.50    --   42.68 -99.00-150.00  103
  2  \w    -30.00  65.00   1.00    7.50    --   42.68 -37.00 150.00   95
  3  \w     16.00 113.00   1.00    7.50    --   42.68  57.00 120.00   97
  4  \w     25.00 109.00   1.00   30.00    --  106.63 -94.00-120.00   84
  5  \w     32.00  69.00   1.00   30.00    --  106.63 -30.00  60.00   37
  6  \w     32.00  69.00   1.00   30.00    --  106.63 -30.00   0.00   37
  7  \w     35.00 122.00   1.00   30.00    --  106.63-125.00-120.00   87
  8  \w     25.00 109.00   1.00   30.00    --  106.63 -94.00 -60.00   84
  9  \w     83.00 158.00   1.00   30.00    --  106.63  30.00-180.00   75
 10  \w     32.00  69.00   1.00   30.00    --  106.63 -30.00  90.00   37
 11  \w     32.00  69.00   1.00   30.00    --  106.63 -30.00  30.00   37
 12  \w     83.00 158.00   1.00   30.00    --  106.63  30.00-150.00   75
 13  \w     35.00  77.00   1.00   30.00    --  106.63 -45.00-150.00   42
 14  \w     36.00 130.00   1.00   30.00    --  106.63 -61.00  90.00   94
;
_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      -0.0383822000
_diffrn_orient_matrix_UB_12      -0.0027737000
_diffrn_orient_matrix_UB_13      0.0335790000
_diffrn_orient_matrix_UB_21      -0.0557505000
_diffrn_orient_matrix_UB_22      0.0089689000
_diffrn_orient_matrix_UB_23      -0.0401928000
_diffrn_orient_matrix_UB_31      -0.0033859000
_diffrn_orient_matrix_UB_32      -0.1152825000
_diffrn_orient_matrix_UB_33      -0.0039703000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            55783
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.341
_diffrn_reflns_theta_min         3.646
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.213
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018)
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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       plate
_exptl_crystal_F_000             3576
_exptl_crystal_recrystallization_method 'from n-hexane by slow evaporation'
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         18506
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0391P)^2^+5.1681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16345
_reflns_number_total             18506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05365a2.cif
_cod_data_source_block           zic297_1
_cod_database_code               7127736
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C85 H117 N6 Ni1 P8 Si2 '
_chemical_oxdiff_usercomment     'from toluene/n-hexane '
_reflns_odcompleteness_completeness 99.95
_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
P008 \\sim C3AB \\sim C3AA: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Sof(H)=Sof(C0AA)=Sof(H0AB)=Sof(H0AC)=Sof(H0AD)=Sof(C1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(H1AD)=1-FVAR(1)
 Sof(H01)=Sof(C02O)=Sof(H4BA)=Sof(HQ)=Sof(HR)=Sof(C02T)=Sof(H8BA)=Sof(HW)=
 Sof(HX)=FVAR(1)
 Sof(HJ)=Sof(C3AB)=Sof(H3AE)=Sof(H3AF)=Sof(H3AG)=1-FVAR(2)
 Sof(H9AA)=Sof(C3AA)=Sof(H3AB)=Sof(H3AC)=Sof(H3AD)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C00V(H00V), C010(H010), C018(H018), C01C(H01C), C01E(H01G), C01F(H01H),
 C01H(H01L), C01I(H01M), C01K(H01Q), C01R(H01), C01R(H), C02J(H9AA), C02J(HJ),
 C02L(H1BA)
4.b Secondary CH2 refined with riding coordinates:
 C02W(H0CA,H3CA), C02X(H1CA,H4CA), C02Y(H2CA,H5CA), C1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00Q(H00Q), C011(H011), C012(H012), C017(H017), C019(H019),
 C01A(H01A), C01B(H01B), C01L(H01R), C01N(H01V), C01P(H01Z), C01S(H0AA),
 C01U(H2AA), C01W(H4AA), C01X(H5AA), C01Z(H7AA), C020(H020), C022(H022),
 C027(H027), C02F(H02Z), C02G(H02), C02P(H5BA)
4.d X=CH2 refined with riding coordinates:
 C00O(H00A,H00B), C023(H02D,H02E)
4.e Idealised Me refined as rotating group:
 C01D(H01D,H01E,H01F), C01G(H01I,H01J,H01K), C01J(H01N,H01O,H01P), C01M(H01S,
 H01T,H01U), C01O(H01W,H01X,H01Y), C01T(H1AA,HA,HB), C01V(H3AA,HC,HD),
 C01Y(H6AA,HE,HF), C021(H02A,H02B,H02C), C024(H02F,H02G,H02H), C025(H02I,H02J,
 H02K), C028(H02L,H02M,H02N), C029(H02O,H02P,H02Q), C02C(H02R,H02S,H02T),
 C02D(H02U,H02V,H02W), C02E(H02X,H02Y,HG), C02H(H8AA,HH,HI), C02K(H0BA,HK,HL),
 C02M(H2BA,HM,HN), C02N(H3BA,HO,HP), C02O(H4BA,HQ,HR), C02R(H6BA,HS,HT),
 C02S(H7BA,HU,HV), C02T(H8BA,HW,HX), C02V(H9BA,HY,HZ), C2(H2A,H2B,H2C),
 C0AA(H0AB,H0AC,H0AD), C1AA(H1AB,H1AC,H1AD), C2AA(H2AB,H2AC,H2AD), C3AA(H3AB,
 H3AC,H3AD), C3AB(H3AE,H3AF,H3AG)
;
_olex2_submission_original_sample_id zic297
_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 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.798