Homoleptic quasilinear metal(i/ii) silylamides of Cr-Co with phenyl and allyl functions - impact of the oxidation state on secondary ligand interactions.
Weller, Ruth; Ruppach, Lutz; Shlyaykher, Alena; Tambornino, Frank; Werncke, C. Gunnar; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10947–10963; doi:10.1039/d1dt01543e

data_7707906
_publ_section_title
;
 Homoleptic quasilinear metal(i/ii) silylamides of Cr-Co with phenyl and
 allyl functions - impact of the oxidation state on secondary ligand
 interactions.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10947
_journal_page_last               10963
_journal_paper_doi               10.1039/d1dt01543e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H56 Mn N2 Si2'
_chemical_formula_sum            'C40 H56 Mn N2 Si2'
_chemical_formula_weight         675.98
_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             2021-06-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-13 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                117.392(4)
_cell_angle_beta                 97.873(4)
_cell_angle_gamma                90.877(5)
_cell_formula_units_Z            4
_cell_length_a                   11.5053(6)
_cell_length_b                   19.5096(13)
_cell_length_c                   19.5355(11)
_cell_measurement_reflns_used    10126
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.50
_cell_volume                     3841.3(4)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
 211 frames, detector distance = 120 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_unetI/netI     0.1343
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38338
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.089
_diffrn_reflns_theta_min         2.504
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm LF focus'
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo LFF X-Ray Tube'
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.7923
_exptl_absorpt_correction_T_min  0.6371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         38338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0859P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18385
_reflns_number_total             38338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           mnl1
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_database_code               7707906
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.841
_exptl_absorpt_special_details
;
The crystal diffracted weakly at angles > 40 \^A\%2(th) 
and was twinned with the twin law -1 0 0 0 0 -1 0 -1 0 
and thus a rather weak data set was obtained.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7535(8)
 0.2465(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C010(H010), C018(H018), C02G(H02P), C02J(H02Q), C013(H013), C01C(H01),
 C02C(H02), C02D(H10)
3.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00P(H00P), C00R(H00R), C00T(H00T), C011(H011), C014(H014),
 C019(H019), C01A(H01A), C01H(H01H), C01K(H01K), C01R(H01R), C01S(H01S),
 C01U(H01U), C01V(H01V), C01W(H01W), C028(H028), C00D(H00D), C00L(H00L),
 C00M(H00M), C00S(H00S), C00V(H00V), C012(H012), C016(H016), C01B(H01Z),
 C01E(H2), C01F(H3), C01I(H4), C01N(H5), C01O(H6), C020(H020), C027(H027),
 C02H(H11)
3.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C01L(H01B,H01C,H01D), C01M(H01E,
 H01F,H01G), C01T(H01I,H01J,H01L), C01Y(H01M,H01N,H01O), C01Z(H01P,H01Q,H01T),
 C021(H02A,H02B,H02C), C025(H02D,H02E,H02F), C02A(H02G,H02H,H02I), C02B(H02J,
 H02K,H02L), C02F(H02M,H02N,H02O), C00U(H00A,H00B,H00C), C017(H01X,H01Y,H),
 C01D(H1,HA,HB), C01P(H7,HC,HD), C01Q(H8,HE,HF), C01X(H9,HG,HH), C022(H02R,H02S,
 H02T), C023(H02U,H02V,H02W), C024(H02X,H02Y,HI), C029(H02Z,HJ,HK), C02I(H12,HL,
 HM), C02K(H13,HN,HO)
;
_shelx_res_checksum              35736
_shelx_hkl_checksum              98865
_olex2_submission_special_instructions 'No special instructions were received'