Synthesis of carbonyl-bridged dibenzofulvalenes and related compounds by rhodium-catalyzed stitching reaction.
Shintani, Ryo; Kishikawa, Shinnosuke; Nakamura, Kimihiro; Tsuda, Tomohiro; Nozaki, Kyoko; Chemical communications (Cambridge, England)  (2019) –; doi:10.1039/c8cc09943j

data_7122770
_publ_section_title
;
 Synthesis of carbonyl-bridged dibenzofulvalenes and related compounds by
 rhodium-catalyzed stitching reaction.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/c8cc09943j
_journal_year                    2019
_chemical_formula_sum            'C36 H43 O P Si2'
_chemical_formula_weight         578.85
_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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-12-08 deposited with the CCDC.
2018-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.636(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.237(4)
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_cell_length_c                   20.841(5)
_cell_measurement_reflns_used    10678
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.2
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_cell_volume                     3143.4(14)
_computing_cell_refinement
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_data_collection
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_data_reduction
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_diffrn_measurement_method       'profile data from \w-scans'
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_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.983
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_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
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_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.302
_diffrn_reflns_theta_min         2.411
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       Block
_exptl_crystal_F_000             1240
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_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
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_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         8879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0468P)^2^+1.5093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7593
_reflns_number_total             8879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09943j2.cif
_cod_data_source_block           ydkr_merge
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7122770
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              46891