Solid‒State Molecular Organometallic Chemistry. Single‒Crystal to Single‒Crystal Reactivity and Catalysis with Light Hydrocarbon Substrates.
Chadwick, Fredrick M.; McKay, Alasdair I.; Martinez-Martinez, Antonio J.; Rees, Nick; Kraemer, Tobias; Macgregor, Stuart Alan; Weller, Andrew; Chem. Sci.  (2017) –; doi:10.1039/C7SC01491K

data_1546504
_publ_section_title
;
 Solid--State Molecular Organometallic Chemistry. Single--Crystal to
 Single--Crystal Reactivity and Catalysis with Light Hydrocarbon
 Substrates.
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01491K
_journal_year                    2017
_chemical_compound_source        SYN
_chemical_formula_moiety         'C32 H12 B1 F24, C29 H54 P2 Rh1'
_chemical_formula_sum            'C61 H66 B F24 P2 Rh'
_chemical_formula_weight         1430.81
_chemical_melting_point          ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-31
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2017-03-23 deposited with the CCDC.
2017-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                91.256(4)
_cell_angle_beta                 90.745(4)
_cell_angle_gamma                96.863(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7894(7)
_cell_length_b                   12.8961(7)
_cell_length_c                   19.8711(8)
_cell_measurement_reflns_used    12342
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     3252.7(3)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27129
_diffrn_reflns_theta_full        45.208
_diffrn_reflns_theta_max         76.624
_diffrn_reflns_theta_min         3.481
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.540
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456.000
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.94
_refine_diff_density_min         -1.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9616
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1052
_refine_ls_number_reflns         12838
_refine_ls_number_restraints     1978
_refine_ls_R_factor_all          0.1525
_refine_ls_R_factor_gt           0.1277
_refine_ls_shift/su_max          0.0083758
_refine_ls_shift/su_mean         0.0008446
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.428E+04 0.715E+04 0.430E+04 0.171E+04 359. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3806
_refine_ls_wR_factor_gt          0.3264
_refine_ls_wR_factor_ref         0.3806
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                9232
_reflns_number_total             12893
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.71
_oxford_diffrn_Wilson_scale      0.25
_oxford_refine_ls_r_factor_ref   0.1525
_oxford_refine_ls_scale          2.38(4)
_oxford_reflns_number_all        12838
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'C:\Users\ASWGroup\Contacts\Deskt At 11:26 on'
_cod_data_source_file            c7sc01491k3.cif
_cod_data_source_block           1propene
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3252.74(13)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C61 H66 B1 F24 P2 Rh1'
_cod_database_code               1546504