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_4348046
_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         'C45 H44 Cu N2 O P2, C F3 O3 S, 3(C4 H8 O)'
_chemical_formula_sum            'C58 H64 Cu F3 N2 O7 P2 S'
_chemical_formula_weight         1115.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0076(5)
_cell_length_b                   15.2895(6)
_cell_length_c                   29.6396(12)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.26
_cell_volume                     5441.5(4)
_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)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            65979
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.091
_diffrn_reflns_theta_min         1.499
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0593 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.8932.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       plate
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 5562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         15968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.1110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                13917
_reflns_number_total             15968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00917_si_005.cif
_cod_data_source_block           dg339_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_database_code               4348046
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.920
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H51C)=Sof(H51D)=Sof(H53C)=Sof(H53D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=1-FVAR(1)
 Sof(H51A)=Sof(H51B)=Sof(H53A)=Sof(H53B)=Sof(C52)=Sof(H52A)=Sof(H52B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C15(H15), C16(H16)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C48(H48A,H48B), C58(H58A,H58B), C49(H49A,H49B), C47(H47A,
 H47B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C50(H50A,H50B),
 C54(H54A,H54B), C51(H51A,H51B), C51(H51C,H51D), C53(H53A,H53B), C53(H53C,H53D),
  C52(H52A,H52B), C52A(H52C,H52D)
3.c Aromatic/amide H refined with riding coordinates:
 C45(H45), C7(H7), C11(H11), C29(H29), C4(H4), C3(H3), C30(H30), C38(H38),
 C6(H6), C39(H39), C35(H35), C32(H32), C23(H23), C33(H33), C5(H5), C21(H21),
 C31(H31), C9(H9), C10(H10), C41(H41), C37(H37), C44(H44), C43(H43), C36(H36),
 C42(H42)
3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'