Copper(I) Complexes of Pyridine-Bridged Phosphaalkene-Oxazoline Pincer Ligands.
Serin, Spencer C.; Pick, Fraser S.; Dake, Gregory R.; Gates, Derek P.; Inorganic chemistry 55 (2016) 6670–6678; doi:10.1021/acs.inorgchem.6b00917

data_4348048
_publ_section_title
;
 Copper(I) Complexes of Pyridine-Bridged Phosphaalkene-Oxazoline Pincer
 Ligands.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6670
_journal_page_last               6678
_journal_paper_doi               10.1021/acs.inorgchem.6b00917
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_moiety
'0.5(C56.98 H61 Cu2 F3 N5 O5 P2 S), 0.5(C F3 O3 S)'
_chemical_formula_sum            'C28.99 H30.5 Cu F3 N2.5 O4 P S'
_chemical_formula_weight         661.51
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                92.416(2)
_cell_angle_beta                 107.396(2)
_cell_angle_gamma                104.977(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3994(11)
_cell_length_b                   11.7624(11)
_cell_length_c                   12.2529(12)
_cell_measurement_reflns_used    9482
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.35
_cell_volume                     1501.8(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33061
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.145
_diffrn_reflns_theta_min         1.756
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0637 before and 0.0509 after correction.
The Ratio of minimum to maximum transmission is 0.9135.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       prism
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.336
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 4053 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         14333
_refine_ls_number_restraints     802
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0507P)^2^+0.0373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.632
_reflns_Friedel_fraction_full    0.710
_reflns_Friedel_fraction_max     0.625
_reflns_number_gt                12028
_reflns_number_total             14333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00917_si_004.cif
_cod_data_source_block           mo_dg318_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C28.99 H30.50 Cu F3 N2.50 O4 P S'
_cod_database_code               4348048
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.785
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1A-O5A \\sim S1-O4 \\sim S1-O5 \\sim S1A-O4A
 with sigma of 0.01
 S1A-O3A \\sim S1-O3
 with sigma of 0.01
 F3A-C57 \\sim F2A-C57 \\sim F1A-C57
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O5A)=Sof(F2)=Sof(F1)=Sof(F3)=Sof(O4A)=Sof(S1A)=Sof(O3A)=1-FVAR(1)
 Sof(S1)=Sof(O3)=Sof(F2A)=Sof(F1A)=Sof(F3A)=Sof(C57)=Sof(O4)=Sof(O5)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C15(H15), C42(H42), C43(H43)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C41(H41A,H41B)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C30(H30), C31(H31), C37(H37), C10(H10), C36(H36), C38(H38), C23(H23),
 C6(H6), C50(H50), C11(H11), C33(H33), C34(H34), C21(H21), C48(H48), C32(H32),
 C4(H4), C5(H5), C3(H3), C7(H7)
5.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C26(H26A,H26B,H26C), C56(H56A,H56B,H56C), C17(H17A,H17B,
 H17C), C27(H27A,H27B,H27C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C52(H52A,
 H52B,H52C), C54(H54A,H54B,H54C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'