Cooperative Ruthenium Complex Catalyzed Multicomponent Synthesis of Pyrimidines
Maji, Milan; Kundu, Sabuj; Dalton Transactions  (2019) –; doi:10.1039/C9DT04040D

data_7701474
_publ_section_title
;
 Cooperative Ruthenium Complex Catalyzed Multicomponent Synthesis of
 Pyrimidines
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04040D
_journal_year                    2019
_chemical_formula_moiety         'C50 H42 N3 O P2 Ru, Cl, C3 H3'
_chemical_formula_sum            'C53 H44 Cl N3 O P2 Ru'
_chemical_formula_weight         937.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-15 deposited with the CCDC.	2019-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 95.099(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   9.806(5)
_cell_length_b                   22.261(5)
_cell_length_c                   19.795(5)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.42
_cell_volume                     4304(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.1038
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43395
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.372
_diffrn_reflns_theta_min         2.066
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6388
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0686 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.8566.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellowish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.110
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         10744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+3.2664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6689
_reflns_number_total             10744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04040d2.cif
_cod_data_source_block           complex_d
_cod_database_code               7701474
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.995
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N007(H007), C010(H010), C011(H011), C012(H012), C013(H013), C014(H014),
 C016(H016), C018(H018), C019(H019), C022(H022), C025(H025), C027(H027),
 C029(H029), C030(H030), C031(H031), C034(H034), C035(H035), C036(H036),
 C037(H037), C038(H038), C039(H039), C040(H040), C041(H041), C042(H042),
 C043(H043), C044(H044), C045(H045), C046(H046), C047(H047), C048(H048),
 C049(H049), C050(H050), C051(H051), C052(H052), C053(H053), C054(H054),
 C055(H055), C056(H056), C059(H059), C060(H060), C061(H061)
2.b Idealised Me refined as rotating group:
 C032(H03a,H03b,H03c)
;
_olex2_submission_special_instructions 'No special instructions were received'