Structural Characterization and Optical Properties of Two Copper(I)-Iodide BODIPY Coordination Polymers
Hassanain, Hawazen; Davies, Edward Stephen; Lewis, William; Kays, Deborah Lorraine; Champness, Neil R.; CrystEngComm  (2019) –; doi:10.1039/C9CE00845D

data_7232990
_publ_section_title
;
 Structural Characterization and Optical Properties of Two
 Copper(I)-Iodide BODIPY Coordination Polymers
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE00845D
_journal_year                    2019
_chemical_formula_moiety         'C29 H25 B F2 N4'
_chemical_formula_sum            'C29 H25 B F2 N4'
_chemical_formula_weight         478.34
_chemical_name_systematic        BhHASOD
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-02 deposited with the CCDC.    2019-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.947(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5686(4)
_cell_length_b                   13.2178(5)
_cell_length_c                   13.7790(5)
_cell_measurement_reflns_used    2253
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.0910
_cell_measurement_theta_min      4.7210
_cell_volume                     2376.12(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            'Agilent Diffraction Titan S2 detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -111.00 -23.00   1.00   30.00    --  -42.83 -57.00 -60.00   88
  2  \w     52.00  79.00   1.00   30.00    --   42.83 -99.00-180.00   27
  3  \w    -27.00  68.00   1.00   30.00    --   42.83 -57.00 120.00   95
  4  \w     32.00  89.00   1.00  120.00    --  107.00 -30.00 120.00   57
  5  \w     37.00  78.00   1.00  120.00    --  107.00 -30.00-150.00   41
  6  \w     40.00  68.00   1.00  120.00    --  107.00 -45.00   0.00   28
  7  \w     88.00 134.00   1.00  120.00    --  107.00  45.00-120.00   46
  8  \w     45.00 118.00   1.00  120.00    --  107.00-125.00  60.00   73
  9  \w    151.00 178.00   1.00  120.00    --  107.00  45.00-120.00   27
 10  \w     38.00  87.00   1.00  120.00    --  107.00 -30.00  60.00   49
 11  \w     56.00  92.00   1.00  120.00    --  107.00-125.00 120.00   36
 12  \w     35.00 123.00   1.00  120.00    --  107.00 -77.00-120.00   88
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0218294000
_diffrn_orient_matrix_UB_12      -0.1108339000
_diffrn_orient_matrix_UB_13      -0.0333450000
_diffrn_orient_matrix_UB_21      0.0324915000
_diffrn_orient_matrix_UB_22      -0.0337834000
_diffrn_orient_matrix_UB_23      0.1112693000
_diffrn_orient_matrix_UB_31      -0.1114890000
_diffrn_orient_matrix_UB_32      0.0120265000
_diffrn_orient_matrix_UB_33      0.0050660000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4769
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.695
_diffrn_reflns_theta_min         4.726
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic orangish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_preparation       'in fobolin on micromount for HMH/NRC'
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0500P)^2^+2.0829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2000
_reflns_number_total             2358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00845d2.cif
_cod_data_source_block           bhasod
_cod_database_code               7232990
_nottingham_internal_coll_name   BHASOD
_nottingham_internal_coll_number 17813
_nottingham_internal_coll_client HMH/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '30.00, 120.00'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxhh4
_nottingham_internal_coll_date   09/08/2018
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 13/08/2018
_nottingham_internal_process_user pcxhh4
_nottingham_internal_solution_date 19/8/2018
_nottingham_internal_solution_user pcxhh4
_nottingham_internal_refinement_date 19/8/2018
_nottingham_internal_refinement_user pcxhh4
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H22 B1 F2 N3'
_chemical_oxdiff_usercomment
'BHASOD #17813 GVB-1559 IN FOBLIN IN MICROMOUNT FOR  HMH/NRC'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.883
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C3(H3), C1(H1), C2(H2), C11(H11), C13(H13)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              75606
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id BHASOD
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.506
_oxdiff_exptl_absorpt_empirical_full_min 0.730