Towards accurate and precise positions of hydrogen atoms bonded to heavy metal atoms.
Woińska, Magdalena; Chodkiewicz, Michał L; Woźniak, Krzysztof; Chemical communications (Cambridge, England) 57 (2021) 3652–3655; doi:10.1039/d0cc07661a

data_7128094
_publ_section_title
;
 Towards accurate and precise positions of hydrogen atoms bonded to heavy
 metal atoms.
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3652
_journal_page_last               3655
_journal_paper_doi               10.1039/d0cc07661a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C27 H55 N9 Ru Si3'
_chemical_formula_sum            'C27 H55 N9 Ru Si3'
_chemical_formula_weight         691.120
_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_Int_Tables_number      14
_audit_creation_date             2021-02-16
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-08 deposited with the CCDC.	2021-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.516(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3827(2)
_cell_length_b                   18.4666(5)
_cell_length_c                   18.9153(5)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.77
_cell_measurement_theta_min      2.46
_cell_measurement_wavelength     0.71073
_cell_volume                     3274.23(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.8798
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.8798
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49277
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.8798
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         36.39
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_correction_T_min  0.8963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1460.215
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
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_refine_diff_density_min         -0.4703
_refine_diff_density_rms         0.1183
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_refine_ls_d_res_low             13.2074
_refine_ls_goodness_of_fit_ref   1.0120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     365
_refine_ls_number_reflns         14045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0120
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+1.3798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                11599
_reflns_number_total             14045
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc07661a2.cif
_cod_data_source_block           NOBBOX_IAM
_cod_depositor_comments
'Adding full bibliography for 7128081--7128095.cif.'
_cod_database_code               7128094
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.03) H1B(0.03) H1C(0.03) H3A(0.017) H3B(0.017) H4A(0.021)
 H4B(0.021) H5A(0.025) H5B(0.025) H7A(0.032) H7B(0.032) H8A(0.025) H8B(0.025)
 H9A(0.021) H9B(0.021) H10A(0.033) H10B(0.033) H10C(0.033) H11A(0.022)
 H11B(0.022) H12A(0.024) H12B(0.024) H13A(0.027) H13B(0.027) H15A(0.026)
 H15B(0.026) H16A(0.023) H16B(0.023) H17A(0.02) H17B(0.02) H19A(0.03)
 H19B(0.03) H19C(0.03) H20A(0.03) H20B(0.03) H20C(0.03) H21A(0.028) H21B(0.028)
 H21C(0.028) H22A(0.021) H22B(0.021) H23A(0.024) H23B(0.024) H24A(0.026)
 H24B(0.026) H26A(0.023) H26B(0.023) H27A(0.023) H27B(0.023) H28A(0.02)
 H28B(0.02) H30A(0.035) H30B(0.035) H30C(0.035)
 Fixed X: H1A(0.1227) H1B(0.2103) H1C(0.137) H3A(0.4803) H3B(0.4223)
 H4A(0.1857) H4B(0.2894) H5A(0.1403) H5B(0.3063) H7A(0.2262) H7B(0.0825)
 H8A(0.3287) H8B(0.1696) H9A(0.092) H9B(0.2149) H10A(0.3737) H10B(0.4986)
 H10C(0.5123) H11A(0.3025) H11B(0.353) H12A(0.1091) H12B(0.1233) H13A(-0.0492)
 H13B(0.0217) H15A(-0.0412) H15B(-0.0613) H16A(0.1489) H16B(0.0224)
 H17A(0.1254) H17B(0.2412) H19A(0.5978) H19B(0.7191) H19C(0.5977) H20A(0.5451)
 H20B(0.6535) H20C(0.4915) H21A(0.5795) H21B(0.5731) H21C(0.7222) H22A(0.8783)
 H22B(0.961) H23A(0.9543) H23B(0.783) H24A(0.9719) H24B(0.8463) H26A(0.7059)
 H26B(0.8497) H27A(0.6362) H27B(0.7285) H28A(0.4827) H28B(0.4838) H30A(0.8932)
 H30B(0.7798) H30C(0.8432)
 Fixed Y: H1A(0.7303) H1B(0.7147) H1C(0.792) H3A(0.8359) H3B(0.7548)
 H4A(0.8001) H4B(0.8334) H5A(0.9218) H5B(0.9418) H7A(1.0194) H7B(0.9784)
 H8A(0.9987) H8B(1.0262) H9A(0.9038) H9B(0.9203) H10A(0.8617) H10B(0.8027)
 H10C(0.8727) H11A(0.482) H11B(0.5293) H12A(0.4981) H12B(0.5843) H13A(0.5594)
 H13B(0.484) H15A(0.5352) H15B(0.6181) H16A(0.5644) H16B(0.6197) H17A(0.7094)
 H17B(0.6834) H19A(0.5324) H19B(0.5602) H19C(0.5064) H20A(0.599) H20B(0.6609)
 H20C(0.6809) H21A(0.9101) H21B(0.921) H21C(0.9276) H22A(0.8606) H22B(0.7846)
 H23A(0.8395) H23B(0.8372) H24A(0.7161) H24B(0.7344) H26A(0.6227) H26B(0.5953)
 H27A(0.5268) H27B(0.5547) H28A(0.5834) H28B(0.6291) H30A(0.8298) H30B(0.8243)
 H30C(0.7522)
 Fixed Z: H1A(0.2861) H1B(0.217) H1C(0.2273) H3A(0.5391) H3B(0.5469)
 H4A(0.5563) H4B(0.6178) H5A(0.5528) H5B(0.5609) H7A(0.4602) H7B(0.4349)
 H8A(0.3538) H8B(0.3336) H9A(0.3224) H9B(0.2684) H10A(0.1964) H10B(0.1979)
 H10C(0.2477) H11A(0.2769) H11B(0.2114) H12A(0.1925) H12B(0.2008) H13A(0.2767)
 H13B(0.3005) H15A(0.4172) H15B(0.3938) H16A(0.4947) H16B(0.5109) H17A(0.4409)
 H17B(0.5002) H19A(0.3828) H19B(0.3325) H19C(0.3021) H20A(0.1863) H20B(0.2136)
 H20C(0.1919) H21A(0.4497) H21B(0.3656) H21C(0.4096) H22A(0.4873) H22B(0.4918)
 H23A(0.6062) H23B(0.6005) H24A(0.6103) H24B(0.6621) H26A(0.6446) H26B(0.6106)
 H27A(0.574) H27B(0.5099) H28A(0.4881) H28B(0.5601) H30A(0.3511) H30B(0.2856)
 H30C(0.3218)
;
_olex2_submission_special_instructions 'No special instructions were received'