A family of cis-macrocyclic diphosphines: modular, stereoselective synthesis and application in catalytic CO2/ethylene coupling
Knopf, Ioana; Tofan, Daniel; Beetstra, Dirk; Al-Nezari, Abdulaziz; Al-Bahily, Khalid; Cummins, Christopher C.; Chem. Sci. 8 (2017) 1463–; doi:10.1039/C6SC03614G

data_1544277
_publ_section_title
;
 A family of cis-macrocyclic diphosphines: modular, stereoselective
 synthesis and application in catalytic CO2/ethylene coupling
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1463
_journal_paper_doi               10.1039/C6SC03614G
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C17 H31 I O P2'
_chemical_formula_weight         440.26
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-09-21 deposited with the CCDC.
2016-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.3520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0682(2)
_cell_length_b                   13.5159(2)
_cell_length_c                   14.7514(2)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.04
_cell_measurement_theta_min      4.40
_cell_volume                     2005.69(6)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37624
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.824
_diffrn_reflns_theta_min         4.395
_diffrn_source                   'fine-focus sealed tube, graphite'
_exptl_absorpt_coefficient_mu    14.023
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_exptl_absorpt_correction_T_min  0.1274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.850
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3398
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_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0522P)^2^+6.4044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2973
_reflns_number_total             3398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc03614g2.cif
_cod_data_source_block           D8_10140
_cod_depositor_comments
'Adding full bibliography for 1544277--1544280.cif.'
_cod_database_code               1544277
_shelx_estimated_absorpt_t_min   0.127
_shelx_estimated_absorpt_t_max   0.541
_shelxl_version_number           2013-4
_shelx_res_checksum              39386