Synthons for carbide complex chemistry.
Reinholdt, Anders; Hill, Anthony F.; Bendix, Jesper; Chemical communications (Cambridge, England) 54 (2018) 5708–5711; doi:10.1039/c8cc03596b

data_7121651
_publ_section_title
;
 Synthons for carbide complex chemistry.
;
_journal_issue                   45
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5708
_journal_page_last               5711
_journal_paper_doi               10.1039/c8cc03596b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C45 H69 Cl N P2 Ru, 6.5(C H Cl3), Cl'
_chemical_formula_sum            'C51.5 H75.5 Cl21.5 N P2 Ru'
_chemical_formula_weight         1633.81
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-02-15 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.149(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7297(10)
_cell_length_b                   19.5656(10)
_cell_length_c                   21.1868(13)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.565
_cell_measurement_theta_min      2.294
_cell_volume                     6916.8(7)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0508
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            139418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.191
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0980 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.8141.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             3324
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.650
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         15246
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0284P)^2^+26.6205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13196
_reflns_number_total             15246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03596b2.cif
_cod_data_source_block           mo_d8v3233_0m-1
_cod_depositor_comments
'Adding full bibliography for 7121645--7121655.cif.'
_cod_original_formula_sum        'C51.50 H75.50 Cl21.50 N P2 Ru'
_cod_database_code               7121651
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.675
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl22(0.5) Cl21(0.5) Cl23(0.5) C52(0.5) H52(0.5)
 Fixed Uiso: H1(0.017) H29A(0.022) H29B(0.022) H13A(0.027) H13B(0.027)
 H31(0.027) H20(0.028) H11(0.025) H19A(0.023) H19B(0.023) H8A(0.02) H8B(0.02)
 H27A(0.022) H27B(0.022) H39A(0.022) H39B(0.022) H41(0.032) H18A(0.025)
 H18B(0.025) H38A(0.024) H38B(0.024) H43A(0.038) H43B(0.038) H3A(0.021)
 H3B(0.021) H10(0.024) H21(0.033) H33A(0.029) H33B(0.029) H9A(0.02) H9B(0.02)
 H35A(0.032) H35B(0.032) H30(0.027) H2A(0.021) H2B(0.021) H37A(0.022)
 H37B(0.022) H4A(0.021) H4B(0.021) H23A(0.035) H23B(0.035) H12(0.025)
 H17A(0.02) H17B(0.02) H40(0.031) H22(0.029) H5A(0.02) H5B(0.02) H42(0.031)
 H7A(0.019) H7B(0.019) H14A(0.029) H14B(0.029) H15A(0.027) H15B(0.027)
 H24A(0.035) H24B(0.035) H28A(0.021) H28B(0.021) H34A(0.031) H34B(0.031)
 H46(0.037) H25A(0.033) H25B(0.033) H48(0.05) H45A(0.035) H45B(0.035)
 H32(0.028) H44A(0.036) H44B(0.036) H47(0.057) H51(0.051) H51A(0.051)
 H50(0.054) H49(0.041) H49A(0.081) H50A(0.056) H52(0.056)
 Fixed X: H1(0.1366) H29A(0.4141) H29B(0.4238) H13A(0.3355) H13B(0.2512)
 H31(0.3053) H20(0.4293) H11(0.3012) H19A(0.193) H19B(0.2828) H8A(0.2887)
 H8B(0.2234) H27A(0.3126) H27B(0.2356) H39A(0.2754) H39B(0.184) H41(0.1734)
 H18A(0.2408) H18B(0.1674) H38A(0.1516) H38B(0.2224) H43A(0.3125) H43B(0.298)
 H3A(0.0733) H3B(0.1554) H10(0.3354) H21(0.2) H33A(0.2485) H33B(0.3339)
 H9A(0.4312) H9B(0.4159) H35A(0.4559) H35B(0.4462) H30(0.3257) H2A(0.1281)
 H2B(0.1466) H37A(0.3693) H37B(0.3875) H4A(0.1545) H4B(0.0716) H23A(0.3256)
 H23B(0.3388) H12(0.5078) H17A(0.399) H17B(0.3847) H40(0.4082) H22(0.2368)
 H5A(0.1407) H5B(0.1212) H42(0.2237) H7A(0.2444) H7B(0.3244) H14A(0.4403)
 H14B(0.4231) H15A(0.4557) H15B(0.4617) H24A(0.147) H24B(0.2073) H28A(0.223)
 H28B(0.2915) H34A(0.4273) H34B(0.443) H46(0.5333) H25A(0.3767) H25B(0.349)
 H48(0.0284) H45A(0.3629) H45B(0.3282) H32(0.5044) H44A(0.1282) H44B(0.1839)
 H47(0.4945) H51(0.1963) H51A(0.2135) H50(0.0305) H49(0.078) H49A(0.0543) H50A(-
 0.0214)
 Fixed Y: H1(0.6565) H29A(0.5463) H29B(0.4844) H13A(0.9889) H13B(0.9662)
 H31(0.4801) H20(0.8363) H11(0.877) H19A(0.7268) H19B(0.6978) H8A(0.7856)
 H8B(0.8433) H27A(0.3919) H27B(0.3994) H39A(0.5925) H39B(0.5684) H41(0.369)
 H18A(0.9044) H18B(0.8533) H38A(0.4492) H38B(0.3976) H43A(0.3498) H43B(0.3687)
 H3A(0.7288) H3B(0.7379) H10(1.0128) H21(0.9142) H33A(0.381) H33B(0.3622)
 H9A(0.8289) H9B(0.7782) H35A(0.3512) H35B(0.3641) H30(0.3165) H2A(0.781)
 H2B(0.8306) H37A(0.4379) H37B(0.5137) H4A(0.6066) H4B(0.6078) H23A(0.8965)
 H23B(0.9293) H12(0.8673) H17A(0.7763) H17B(0.8566) H40(0.4331) H22(0.7075)
 H5A(0.4989) H5B(0.5316) H42(0.5642) H7A(0.9248) H7B(0.9215) H14A(0.9002)
 H14B(0.821) H15A(0.9547) H15B(0.9824) H24A(0.8014) H24B(0.8181) H28A(0.4983)
 H28B(0.5557) H34A(0.5262) H34B(0.4506) H46(0.6844) H25A(0.7231) H25B(0.77)
 H48(0.4445) H45A(0.544) H45B(0.4879) H32(0.4625) H44A(0.4804) H44B(0.4495)
 H47(0.1543) H51(0.1464) H51A(0.1388) H50(0.6895) H49(0.2818) H49A(0.2388)
 H50A(0.3276)
 Fixed Z: H1(0.2547) H29A(0.1739) H29B(0.2234) H13A(0.0872) H13B(0.1123)
 H31(0.0121) H20(0.4523) H11(0.0489) H19A(0.3639) H19B(0.3681) H8A(0.1221)
 H8B(0.1341) H27A(0.2222) H27B(0.1731) H39A(0.3541) H39B(0.3426) H41(0.3879)
 H18A(0.3382) H18B(0.3466) H38A(0.3029) H38B(0.2882) H43A(0.3775) H43B(0.4494)
 H3A(0.1802) H3B(0.1463) H10(0.1974) H21(0.4434) H33A(0.0566) H33B(0.0312)
 H9A(0.2517) H9B(0.1925) H35A(0.1098) H35B(0.1836) H30(0.1349) H2A(0.2725)
 H2B(0.2151) H37A(0.3059) H37B(0.3318) H4A(0.1311) H4B(0.1649) H23A(0.4997)
 H23B(0.4319) H12(0.1677) H17A(0.355) H17B(0.3442) H40(0.4165) H22(0.472)
 H5A(0.1761) H5B(0.2426) H42(0.4529) H7A(0.2247) H7B(0.2711) H14A(0.0688)
 H14B(0.082) H15A(0.2324) H15B(0.1617) H24A(0.4519) H24B(0.5123) H28A(0.0982)
 H28B(0.0989) H34A(0.0587) H34B(0.033) H46(0.3783) H25A(0.4615) H25B(0.518)
 H48(0.6962) H45A(0.4441) H45B(0.4901) H32(0.1376) H44A(0.4146) H44B(0.4725)
 H47(0.2949) H51(0.3257) H51A(0.332) H50(0.4397) H49(0.7014) H49A(0.1945)
 H50A(0.5625)
;
_shelx_res_checksum              97114
_olex2_submission_special_instructions 'No special instructions were received'